1111Total Synthesis of Ketamine [Type the document subtitle] [Type the abstract of the document here. The abstract is typically a short summary of the contents of the document. Type the abstract of the document here. The abstract is typically a short summary of the contents of the document.] Total Synthesis of Ketamine While there’s 11 steps in the synthesis, its longitude is explained by the fact that all the precursors and even some reagents are made from scratch, employing user-friendly techniques and equipment (in fact, a need for vacuum is mentioned only once, and even that is for the removal of solvent); as well as only easy-to-get reactants. Still the synth is obviously for the skilled only; for one thing, it involves making a Grignard. There is a potential possibility to use zinc organic compounds instead (discussed in detail below) which is much cheaper and easier technically. Also there is added an alternate preparation of o-chlorobenzonitrile Experimental sodium nitrite Sodium nitrate is also synthesized industrially by neutralizing nitric acid with soda ash 2 HNO3 + Na2CO3 → 2 NaNO3 + H2O + CO2 nitric acid HNO3 Molar mass 63.01 g mol−1 / Density 1.5129 g cm−3 soda ash Molar mass 105.9784 g/mol (anhydrous) 124.00 g/mol (monohydrate) 286.14 g/mol (decahydrate) Density 2.54 g/cm3 (anhydrous) 2.25 g/cm3 (monohydrate) 1.51 g/cm3 (heptahydrate) 1.46 g/cm3 (decahydrate) 756 GRAMS (498 ML,S) NITRIC ACID HNO3 636 GRAMS (246 ML,S) SODIUM CARBONATE (SODA ASH) ……………………………………………………………………………………. 1. o-Chlorobenzoic acid • • • • Anthranilic acid 13,7g HCl (conc., d=1,19) NaNO2 8g ( sodium nitrite) CuCl 10g (Copper Chlorides) 13,7 grams anthranilic acid is stirred in a glass beaker in 40ml,s destiled water, 28ml,s hydrochloric acid HCl and 20 grams ice. With constant stirring and cooling there's added 8 grams sodium nitrite NaNO2 in 40ml,ss water. Thus obtained clear solution of diazonium salt is very slowly added with stirring into a soln. of 10 grams copper chloride CuCl in 25 grams hydrochloric acid HCl conc. A vigorous evolution of nitrogen is observed. When the rxn ends, the ppt is filtered, washed with cold water and reprecipitated from aq. Sodium carbonate Na2CO3. The product represents fine crystals and melts at 140-141°C. o-Bromobenzoic acid can be obtained in an analogous manner, substituting copper chloride CuCl for CuBr. CuBr (ver) Preparation of Copper Chlorides I prepared cuprous chloride by mixing copper wire, CuCO3 and a excess of commercial 20 % hydrochloric acid HCl and warming it near boiling point until all copper was dissolved. It was the deposition of a white powder (cuprous chloride). This product can't be dried because it oxydizes quickly, it was washed with water. Normal reaction is with copper wire or powder, cupric chloride CuCl2 and hydrochloric acid HCl, but I had then CuCO3. CuCO3 (ver) Also cupric chloride was prepared by reacting a solution of CuCO3 with an slightly excess of hydrochloric acid HCl, then evaporating water and finally, when product starts to turn brown, air dried to give a hydrate form. copper wire CuCO3 20 % hydrochloric acid HCl solution --------------------------------------------------------------------------- 2. o-Chlorobenzonitrile Preparation A. (RCOO)2Zn + Pb(SCN)2 = 2 RCN + ZnS + PbS + 2 CO2 The best results are obtained when a zinc salt is employed instead of free acid. This rxn is unsuitable for amino-, nitro- and oxy- acids, but can bee used for bromo- and chlorobenzoic acids. To a hot soln of 50 grams sodium hydroxide NaOH in 400ml,s water there's added 195 grams o-chlorobenzoic acid. Carefully neutralize with ammonium hydroxide NH3 or sodium bicarbonate NaHCO3 and add with heating 105 grams (~5% excess) zinc sulphate ZnSO4 in 400 ml,s destiled water. The precipitated salt is dried for prolonged time at 200°C and mixed intimately with 205 grams (Lead(II) thiocyanate) Pb(SCN)2. The mixture is coffee ground and dried at 120-140°C for a prolonged time, then heated on open flame - the mixture melts and gases are evolved. At 250-255°C distillation begins.... The collected product is redistilled.. Heat the nitric acid to boiling.... …………………………………………………………………………………………………………. This one doesn't require a prolonged drying...c). mp 53-57°C.... yield 36 grams (80% of theory). 1-42.....) of concentrated nitric acid.... Once the reaction has started....... ADIPIC ACID Into a 3-litre three-necked flask...Distilled nitrile is treated with hydroxide de ammonia NH4OH. add 500 g... but the duration of dryings makes the method quite time-consuming... an explosion may result if cyclohexanol is allowed to accumulate in the acid.. Since oxides of nitrogen are evolved in the subsequent oxidation... gr... may have to be replaced before the operation is complete... I’ll post it later separately......... Preparation B.....but since this is a very good route to subst’d benzaldehydes from benzoic acids.. o-Bromobenzonitrile 50 grams o-Bromobenzamide and 35 grams (25 grams =theory) sulfaminic (sulfamic) acid is thoroughly mixed and heated in a Wurtz flask.... The rxn usually takes place within 30-60 mins..... steam-distilled and salted out.. if the addition of the secondary alcohol is too slow..//.. l. this can bee simplified yet more. bp 251-253°C As I found recently. which are attacked by nitrous fumes........... of cyclohexanol through the dropping funnel at such a rate that all is introduced in 4-5 hours ......... place 1900 ml... which is over at 285-295°C (takes approx. a mechanical stirrer (1) and a long reflux condenser.. mp 43-46°C. by forming benzamides in situ from the corresponding acid and urea.............. add a few drops of ciclohexanol and make certain that these are acted upon by the acid before adding more .. Sulfaminic acid is dirt cheap and can be acquired without causing any suspicion.... the reaction should be carried out in a fume cupboard.. 8...... set the stirrer in motion. (2700 g. the corks (2)............ sp... Keep the reaction mixture at the boiling point during the addition of the cyclohexanol and for a further period of about 15 minutes in order to complete .... Electrowinning processing leaches zinc from the ore concentrate by sulfuric acid:[81] ZnO + H2SO4 → ZnSO4 + H2O . or the oxides of nitrogen are led by a tube from the top of the condenser to a water trap (Fig.. 1............. Yield 137 grams (80%). ……………………………………………………………………………………………... fitted with a dropping funnel.5-2 hrs).. bp 232°C....... . Filter on a large sintered glass funnel.Bp 130-140°C at 7mmHg...... if one is to use pre-made Calcium oxide Ca or Ba adipinate.. the adipic acid crystallises.. The rxn is heated to 280 °C....... which lasts about 1-2 hrs... is 400 g....... Ca(OH)2 (ver) Ba adipinate (ver) .. The yield of recrystallised adipic acid...p..... the mixture initially melts and then the distillation takes place................ Aluminium isopropoxide Al(i-PrO)3 . Notes: • • Ca(OH)2 may bee substituted for barium hydroxide Ba(OH)2 without much loss in the yield... of concentrated nitric acid .. and wash with 200 ml... 3........ Dry with magnesium sulphate MgSO4.. ....the oxidation.... m... upon cooling.... filter and wash as above... of cold water.. 152°..... (3)...... Cyclopentanone 100 grams adipic acid and 10 grams barium hydroxide Ba(OH)2 is intimately mixed and placed into a flask with a thermometer.. no temp control is necessary. concentrated nitric acid ………………………………………………………………………………………………………...s concentrated nitric acid cyclohexanol destiled water.. mp 118°C... Recrystallise the crude acid from 700 ml. Yield: 51 grams (89% of theory).. The hot distillate is saturated with sodium chloride NaCl. Pour the warm reaction mixture into a beaker ..................... collecting the fraction boiling at 128-130 °C..................... 4.s 700 ml....... 2700 grams 500 grams 200 ml.. the upper layer is decanted and distilled.... collecting the fraction boiling at 137-140°C.S SODIUM HYDROXIDE (781. when it is stopped. 5. The mixture is heated. Cyclopentanol Into a 250 ml. heating is continued until almost full dissolution of aluminium metal Al (5-7 hrs). Drying with magnesium sulphate MgSO4. which causes acetone with some water to distill off. The distillation is ended when the temp of the vapors rises to ~85°C. sometimes even cooling's needed. isopropanol IPA (commercial reagent grade isopropanol IPA was used without any drying) and 0. The upper layer is decanted and distilled. Sodium sulfate synthesis it can be made by the rxn of sulphuric acid H2SO4 with sodium hydroxide NaOH acid+base----> salt +water 2 NaOH+ H2SO4-----> Na2SO4+ 2 H2O so you can mix (2M NaOH) and (1M H2SO4) NaOH Molar mass 39.13 g/cm3 H2SO4 (100%) (1.s (Macrophage inflammatory protein-1β (MIP-1β) is a CC chemokine CCl4 (CAREFUL! Extremely toxic!) and heating continued until hydrogen gas H2 evolution starts. Yield: 47grams (94%) ……………………………………………………………………………………………….58 GRAMS NAOH) . The ppt inside the flask is carefully decomposed with 50% sulfuric acid H2SO4 until acidic and saturated with sodium chloride NaCl.s (51 ml.Into a 250 ml.s isopropanol IPA and the solt from the previous prep.8356 g·cm-3 ) ( 98. After the rxn subsides.s in theory) abs.5 ml.s RBF equipped with an efficient reflux condenser there's added 6 grams Al foil.9971 g mol-1 / Density 2. but you have to double the amount of NaOH then heat the product to evaporate the water and ur left with Na2SO4 which is of course sodium sulphate 530 ML.. In the beginning of boiling 0. ………………………………………………………………………………………………. The rxn is gently heated. The obtained solution is immediately used as is in the following preparation..S SULfURIC ACID H2SO4 (975 GRAMS H2SO4) 367 ML.s (50 grams) cyclopentanone in 50ml.08 g/mol) or same concentration of both. which contains about 40 grams Al isopropoxide. 70 ml.1 grams sulfuric acid HgSO4.s RBF equipped with a 15 cm Vigreux column and distilling condenser there's added 53 ml. Hydrobromic acid 220 grams of KBr (potassium bromide) 200 ml. you should substract one degree when reading your thermometer. Add a few boiling chips. The acid obtained is approximately 47. The rxn is left for 24hrs with vigorous stirring. in order not to form any free bromine.s of distilled water 90 ml. Dryed with magnesium sulphate MgSO4. HBr. collecting the fraction between 137-138°C. Cyclopentylbromide In a flask there’s mixed 47ml.] Even purer HBr can be obtained by redistilling and collecting the portion boiling at 126 °C. Yield = 58 grams (74%) ……………………………………………………………………………………………… Hydrobromic acid H2SO4 + KBr --> KHSO4 + HBr 220 grams of KBr (potassium bromide) or 190 gams of NaBr (sodium bromide) is dissolved in 200 ml.s of concentrated sulphuric acid H2SO4 is chilled in the ice bath and then slowly added to the chilled bromide solution being sure not to allow the temperature to rise above 75°C. The solution is then placed in a 1000 ml. If it reads 100 °C. you should add one degree when reading your thermometer. 90 ml. but when the temperature reaches 125°C replace the receiving flask with a clean flask. Monitor the temperature as it will continue to rise to 126°C and remain there steadily until the constant boiling solution has distilled over. Start a flow of water through the condenser and heat with flame through a wire gauze. The solution is cooled to room temperature and the K2SO4 ( by product) that was formed is filtered out.s of distilled water and chilled in an ice bath. If it reads say 99 °C. If it reads say 101°C.s (45grams) cyclopentanol and 60ml. [It is important to know the correct temperature in order to collect the proper fraction.………………………………………………………………………………………………………………………… 6.5% HBr with a density of 1.s water and the lower organic phase is separated and washed with water twice. 10 grams sodium sulphate Na2SO4 is added.s of concentrated sulphuric acid H2SO4 K2SO4 by product Iodine Crystals or 190 grams of NaBr (sodium bromide) . After that it’s diluted with 200 ml.49g/ml. To calibrate the thermometer first boil water in the apparatus and note the temparature. Water will distill over first. When the temperature begins to drop stop the distillation.s boiling flask in a simple distillation apparatus. then the thermometer reads correctly. Distill.s (90 grams) 48% aq. just ask again. and at the bottom there may bee left some unreacted magnesium Mg as a dark-grey powder.. with a purifying step. 8 . The mixture instantly becomes cloudy from magnesium iodine MgI.s THF (kept over potassium hydroxide KOH. From the addition funnel there’s dripped 55 grams (40 ml. Cyclopentyl magnesium bromide Into a 250 ml. The result is an organic solution of iodine. the solvent may be allowed to evaporate at room temperature. prior to the rxn 150 ml. 9 grams of fine magnesium Mg turnings is added followed by some iodine crystals.Add then the hydrogen peroxide solution You will observe the formation of a brown color due the iodine liberation from the iodine ions present 6. The rxn is usually over in an hour.s Evaporating dish Hydrogen peroxide 20 volume Tetrachloromethane or dichloromethane Distilled water 1M solution of Sulphuric acid Supply of ribbon seaweed (Laminaria) . 3 . Hope that satisfies you.Filter the suspension 4 . about a spoonful.In order to obtain crystals .s of distilled water in a beaker.s) cyclopentyl bromide in 100 ml. Magnetic stirring is commenced. If you need a more sophisticated method. and heat the suspension until it boils. The apparatus is flushed with argon and a gentle stream of gas is left flowing in. 7.Add to the ash 20 ml. it is accompanied by precipitation of a white jelly-like mass. by placing it in an evaporating dish in a fume cupboard.Acidify the filtered with Sulphuric acid solution 5 . 250 ml. . ……………………………………………………………………………………………….that you can obtain a a biological supply store or from the sea shore Procedure (You must work at a fume cupboard) 1-Collect and dry about a dozen 50 cm lenghts of the seaweed and heat them strongly on a tin recipient until they are reduced to ash.You will need: Bunsen burner and asbestos square (or a hot plate) Tripod and tin lid Beaker.s tetrahydrofuran THF so that the solt boils smoothly. 2. It will result crystals of iodine or rather gray-black brilliant flakes. probably it will reduce a quite small quantity. addition funnel and inert gas inlet there’s placed 50 ml.s refluxed over 30 grams CaO for 6hrs and distilled).s Separating funnel 100 ml.s three-necked flask equipped with a reflux condenser.Transfer the mixture to a separating funnel 7 -Extract the Iodine with tetrachloro methane or other solvent. if the rxn conditions are made harsher (gentle reflux instead of RT?). Haloanhydrides generally are the best species for coupling with metalorganics. Nitriles are not bad as electrophiles. Hydrochloric acid HCl acid to NH3 amoniaco (aq) or NH4OH. tetrahydrofuran THF can be dried with CaO. don't add NH3OH(aq) to HCl because it can create a highly exothermic reaction which might damage you.CaO (ver) Usage of tetrahydrofuran THF instead of ether is preferred since the rxn in it proceeds better and faster (tetrahydrofuran THF is a more specific solvent for Grignards) . Bis-dicyclopentyl zinc is conveniently made from the corresponding bromide." …………………………………………………………………………………………………………… Ammonium chloride crystals add dil. Notes on the possible usage of Zn-organics: ". NH4OH + HCl --> NH4Cl(aq) + H2O so according to this balanced equation do the amount calculations and add them in 1 : 1.esp. they would work equally well here . o-Chlorophenyl cyclopentyl ketone . while for ether . the yield is better as well.sodium metal is usually employed. And o-chlorobenzoyl chloride can be easily prepared from o-chlorobenzoic acid (obtained in Step 1) and PCl5 or some such. then heat the solution until you get the white crystals. no need to make iodide here. so it is possible that despite smaller reactivity of ZnR2 compounds. PARA ?????????????? DE AMMONIUM CHLORIDE CRYSTALS 1 LITRO ACIDO CLORIDRICO 1 LITRO DE AMONIACO 8. water will be vapourised and you'll be left with the crystals.. ZnR2 (ver) What one CAN say for sure-is that the rxn with ZnR2 will go just fine if one is to use ochlorobenzoyl chloride instead of benzonitrile. Besides. until neutral. Then 30ml. with addition of some conc. and stirred at RT for 30mins. Manufacture Of Ethyl Iodide This is usually prepared by the action of iodine on alcohol in the presence of red phosphorus.s triethylamine (17g/23mL is required for neutralization of potassium bromine HBr. It is then poured into a mixture of ice / ammonium chloride NH4Cl. and the mixture allowed to stand for twenty-four hours. and then with water. The ketone partially floats. The solvent is removed. ………………………………………………………………………………………………………. and then 10 parts of iodine are added gradually. This may lead to some preciptation of the bromoketone. after which treatment it is dried over fused calcium chloride. (1-hydroxy-cyclopentyl)-(o-chlorophenyl)-N-methylketimine 45 grams of the above bromoketone is dissolved in 50 ml. It’s extracted with benzene. partially goes to the bottom. much as described under "ethyl bromide. giving 30 grams (80%) of methylketimine. The crude product is purified by washing first with dilute solution of sodium hydroxide.s (Macrophage inflammatory protein-1β (MIP-1β) is a CC chemokine CCl4 and with cooling in snow it is added into a solt of 48 grams dioxane dibromide in 50 ml. and iodine 23. Thus Wurtz indicates phosphorus 7 parts. but a 2x excess is used). which stays in (Macrophage inflammatory protein1β (MIP-1β) is a CC chemokine CCl4. ………………………………………………………………………………………………… 10. dried thru sodium hydroxide NaOH. According to Beilstein. The solt is then saturated with 5 grams methylamine. The rxn is left for 1 day and the solvents are removed under aspirator vacuum. 9. add there 50 ml.s dioxane. alcohol.To the thus obtained Grignard solt there’s added 48 grams o-chlorobenzonitrile and the mixture is stirred for 3 days at RT. The yields fluctuate. . whilst Frankland used these in the ratio of 7: 35: 14. obtained by dripping a saturated solt of 15 grams methanolic solution of methylamine hydrochloride MeNH2·HCl onto 10 grams sodium hydroxide NaOH. aq.sdestiled water are added and the solt is washed with sodium carbonate Na2CO3 aq. but rarely drop below 55%. alcohol 35. and the ethyl iodide distilled off. 1 part of red phosphorus is placed in a retort with 5 parts of 90 per cent. Ammonia hydroxide NH3 and left at ambient temp until all ice melts. giving 47 grams (85%) of the bromoketone. ……………………………………………………………………………………………….s benzene." Various proportions of ingredients have been recommended. and redistilled if necessary. alpha-Bromo-(o-chlorophenyl)-cyclopentyl ketone 40 grams ketone is dissolved in 70 ml. At the end of that period the retort is warmed. and dried. and obtains about 570 grams of the iodide for 500 grains of iodine used. and the last stages conducted slowly until experience has been gained. and the operations repeated until the whole 500 grams of iodine have been worked up. round-bottomed flask. The flask is then connected up. When the reaction is completed. When all the iodine has been dissolved. Methyl iodide can be prepared in a similar manner. of the theoretical yield. The alcohol and the two kinds of phosphorus are placed in the flask. he has devised an arrangement to shorten the time and labour. A wide-mouthed. separated from the aqueous layer. a small quantity of water is poured down the condenser to destroy any phosphonium compounds which may have been formed. The chief precaution to be taken is the proper regulation of the temperature when the final charge of iodine is being dealt with. dissolves more or less of this iodine. The arrangement is such that when alcohol placed in the flask is boiled. The flask is then cooled. 250 of alcohol. These are connected at the top with a tube which passes to a reflux condenser. the heating is continued until there is no longer any coloration in the liquid due to iodine. The flask is then detached. 30 Grams red phosphorus 30 Grams yellow phosphorus 250 Grams alcohol iodine 500 grams iodine crystals (optional) (synthesis) (super mercados) (synthesis) ……………………………………………………………………………………………………. after which the heating is re-commenced. is practically pure ethyl iodide. serving as receptacle for the iodine and a wide side-tube.Walker1 recommends the use of both red and yellow phosphorus. Too much heat should be avoided. and heated on a water-bath to boil the alcohol. This consists essentially in an adaptation of the principle of the Soxhlet extractor to the purpose. and 30 of red phosphorus. Distillation should not be allowed to proceed too rapidly. and the liquid distilled off by means of a water-bath. and a fresh charge of iodine placed in the adapter. falls back on the iodine contained in the adapter. or 93 per cent. is condensed in the reflux condenser. and carries it down into the flask. carries a two-holed cork into which are fitted an adapter. after being washed with water. 30 of yellow phosphorus. as much heat is disengaged during the reaction. with a few fragments of porous tile to prevent bumping. in equal quantities. Diethylamine and triethylamine . To obtain about 550 grams of ethyl iodide the ingredients used are 500 grams of iodine. The distillate. As the dissolving of the iodine in the alcohol is tedious. where the solution of iodine in alcohol reacts with the phosphorus present. up which the alcohol vapour passes.. of about 1 litre capacity. its vapour passes up the side tube. and 100 grams of the iodine are packed tightly in the adapter. Then the pipe is returned to the tub of ice water. . yielding the freebases of all. After most of the ammonia has evaporated. the contents of the pipe should be emptied into a beaker. slowly at first to prevent it from boiling over. The bottom of the pipe is secured by screwing the cap on over threads coated with Teflon tape. add 175 ml. Then liquid ammonia is added to the pipe. and the ammonia is allowed to slowly evaporate away. In a 3-inch diameter pipe. and is then filled about 1/2 full of rubbing alcohol.s of liquid ammonia is called for. Now secure the top of the pipe by screwing on the cap tightly over Teflon tape. This neutralizes the HI (ver) in the mix. A really nice touch would be to have all the pieces plated with a half-thousandths-inch of electroless nickel. attaching plastic tubing to the valve. and fine threads are cut into each end so that a cap may be screwed onto each end. This is best done by inverting a cylinder of liquid ammonia. The pipe is now moved into a tub of ice water. The foul substance is a mixture of ammonia. but the plater may think you are constructing a pipe bomb when he sees the pipe and caps. This will take overnight. The extracts should be filtered. as its melting point is about 100 °C below 0 °C.The reaction which produces diethylamine also yields as byproducts ethylamine and triethylamine The relative amounts of each compound produced depends upon the molar ratio of the two starting materials. A rural setting with beaucoup ventilation is more proper. When 30 minutes have passed from the first shaking. and then to this solvent dry ice is added. Toluene is chosen because it is available at the hardware store. a roughly even split occurs. Next. and returned to the ice water. diethylamine. This mixture should be extracted several times with toluene.s of destiled water. and slowly add with stirring 90 grams of sodium hydroxide dissolved in 100 ml.s of ethyl iodide to the pipe. This will be done here. ethlyamine. and raise great plumes of stink. The pipe is then nestled into a Styrofoam cooler. It will not freeze. This shaking should be repeated a few times at 5-minute intervals. The best route to follow is to cool this mixture in. the pipe should be returned to the dry ice bath and allowed to cool. the cap on the top of the pipe is loosened. and the hydriodides thereof. A section of clean steel pipe 2 or 3 inches in diameter is obtained. Use of only a little ethyl iodide favors the formation of mostly ethylamine Use of a lot of the ethyl iodide favors the formation of triethylamine Somewhere in the middle. and its boiling point is higher than any of the amines. triethylamine. This is not an operation to be done in a residential neighborhood. then more rapidly. and cracking open the valve to feed the liquid into the pipe. and let it cool down. and allowed to sit in this ice water for 45 minutes to an hour to warm up to 0 °C. it should be shaken to mix the two reactants. and dried over sodium hydroxide pellets. The top of the pipe should be covered to prevent frost from forming inside the pipe as it cools down. that plus the ethyl iodide will fill it half full. as the fumes are tremendous. Welding may also be used. When the pipe has warmed to 0 °C. When the pipe has cooled. About 525 ml. This product can't be dried because it oxydizes quickly. when product starts to turn brown.The toluene extracts should then be transferred to a flask. It was the deposition of a white powder (cuprous chloride). Ketamine 10 grams of methylketimine is dissolved in 100ml. but I had then CuCO3. Absolute freedom from water in the product can be assured by letting the crude distillate sit over a few chips of potassium hydroxide KOH for a few hours prior to the final distillation. Solvent is removed giving the product as an oil that quickly crystallizes.s liquid ammonia hydroxide 5400 6000 grams sodium hydroxide ml. Preparation of Copper Chlorides I prepared cuprous chloride by mixing copper wire.s destiled water (for extraction) Toluene 2 kilos potassium hydroxide KOH Bomb nickel coted ………………………………………………………………………………………………….s. The diethylamine fraction should be collected over a 20-degree range centered on 55 °C. The yields are close to quantitative.s ethyl iodide 31500 ml. CuCO3 and a excess of commercial 20 % hydrochloric acid HCl and warming it near boiling point until all copper was dissolved. air dried to give a hydrate form. it was washed with water.s undecane and boiled at 195°C for 3-4hrs. ……………………………………………………………………………………………. It can bee purified by recrystallization from pentane/ether or hexane/ether. 11. and triethlyamine distills at 89 °C. CuCl2 and hydrochloric acid HCl. diethylamine distills at 55 °C. and the mixture fractionally distilled through an efficient column Ethylamine distills at 16 °C. The yield of diethylamine is about 40 ml. then evaporating water and finally. . and this fraction then redistilled to get the pure product. 10500 ml. Normal reaction is with copper wire or powder. Also cupric chloride was prepared by reacting a solution of CuCO3 with an slightly excess of hydrochloric acid HCl. Acidic extract is basified and extracted with dichloromethane DCM. Ketamine is extracted with 20% hydrochloric acid HCl. .S) NITRIC ACID HNO3 (NaNO2 sodium nitrite) 636 GRAMS (246 ML.19) 160 grams NaNO2 (sodium nitrite) 756 GRAMS (498 ML.s 400 ml. d=1.s destiled water (chines) (synthesis) (synthesis) (super market) (ver synthesis) (ver synthesis) (ver) 3900 grams o-chlorobenzoic acid NH3 or NaHCO3 (sodium bicarbonate) 2100 grams (~5% excess) ZnSO4 (ZINC SULFATE) 4100 grams Pb(SCN)2 (Lead(II) thiocyanate) NH4OH ( Hidróxido de amônio) .s 40 g 5% hypochlorite solution destiled water phthalimide Hydrochloric acid HCl (conc.--------------------------------------------------------------------------- Total synthesis ( 100 grams ) o-Chlorobenzoic acid 274 grams Anthranilic acid 200 ml.S) SODIUM CARBONATE (SODA ASH) (NaNO2 sodium nitrite) (synthesis) (anthranilic acid synthesis)(lojas de piscinas) (anthranilic acid synthesis) (anthranilic acid synthesis) (ebay ver) (chines) (synthesis) 200 grams CuCl (Copper Chlorides) 300 grams copper wire (synthesis) (Copper Chlorides (Copper Chlorides synthesis) (Copper Chlorides synthesis) synthesis) CuCO3 20 % hydrochloric acid HCl solution o-Chlorobenzonitrile 1000 grams sodium hydroxide NaOH 16000 ml. s 2 isopropanol IPA (isopropanol) (super market) (conservar e restaurar .Sulfaminic acid ( ver synthesis) o-Bromobenzonitrile 1000 grams o-Bromobenzamide 700 grams (500 grams sulfaminic (sulfamic) acid (synthesis) ( ver synthesis) Cyclopentanone 2000 grams adipic acid ( synthesis) 2700 grams 500 grams 200 ml.s CCl4 (carbon tetrachloride) . farmacias) (conservar e restaurar) (ver) grams HgSO4 (sulfuric acid) 100 ml.s 700 ml.s concentrated nitric acid cyclohexanol destiled water concentrated nitric acid (adipic acid synthesis) (adipic acid synthesis) (adipic acid synthesis) (adipic acid synthesis) 200 grams Ba(OH)2 (Barium hydroxide ) Sodium chloride NaCl (table salt) MgSO4 (magnesium sulphate) ( ebay) (super market) (farmacias) Aluminium isopropoxide 120 grams Al foil 1400 ml. s 1200 ml.S SULfURIC ACID H2SO4 734 ML.s (900 grams ) cyclopentanol (1800 grams) 48% aq.s (1000 grams ) cyclopentanone 1000 ml.s tetrahydrofuran Thf KOH (Potassium hydroxide) (ver where to get) (ebay) (ebay) 600 grams CaO (Calcium oxide) .s IPA (isopropanol) 800 grams Al isopropoxide (synthesis) (famacias .s distilled water ) 90 ml. HBr (hydrobromic acid) (synthesis) (synthesis) 220g KBr (potassium bromide) or 190g NaBr (sodium bromide)((hydrobromic acid synthesis) 200 ml.S SODIUM HYDROXIDE 4000 ml. conservar e restaurar) (synthesis) Cyclopentylbromide 940 ml.s destiled water MgSO4 (magnesium sulphate) Cyclopentyl magnesium bromide 1000 ml.s concentrated H2SO4 ) (hydrobromic acid synthesis) ((hydrobromic acid synthesis) ( by product hydrobromic acid synthesis) (synthesis) (sodium sulphate synthesis) (sodium sulphate synthesis) (synthesis) (farmacias) K2SO4 2000 grams Na2SO4 (sodium sulphate) 1060 ML.Cyclopentanol 1060 ml. s tetrahydrofuran THF (solvent) (cylinder or generator (ver) (synthesis) (ver where to get) o-Chlorophenyl cyclopentyl ketone 960 grams o-chlorobenzonitrile NH4Cl (ammonium chloride) (synthesis) (synthesis) (Ammonium chloride synthesis) (Ammonium chloride synthesis) (chines farmacias) 1 LITRO ACIDO CLORIDRICO 1 LITRO DE AMONIACO NH3 (ammonia hydroxide) alpha-Bromo-(o-chlorophenyl)-cyclopentyl ketone 800 grams o-Chlorophenyl cyclopentyl ketone 1400 ml.s CCl4 (carbon tetrachloride) (synthesis) (ver) (ver) 960 grams dioxane dibromide .that you can obtain a a biological supply store or from the sea shore ( iodine crystals synthesis) argon gas 1100 grams ( 800 ml.180 grams Mg turnings iodine crystals Hydrogen peroxide 20 volume Tetrachloromethane (ver) or dichloromethane Distilled water 1M solution of Sulphuric acid (ver where to get) (synthesis) ( iodine crystals synthesis) ( iodine crystals synthesis) ( iodine crystals synthesis) ( iodine crystals synthesis) Supply of ribbon seaweed(Laminaria) .s ) cyclopentyl bromide 2000 ml. s dioxane (solvent) destiled water Na2CO3 (sodium carbonate) (where to buy) (synthesis) (super market) 1-hydroxy-cyclopentyl)-(o-chlorophenyl)-N-methylketimine 900 grams alpha-Bromo-(o-chlorophenyl)-cyclopentyl ketone 1000 ml.s ethyl iodide 31500 ml.s 1000 ml.s 600 ml.s destiled water Toluene (for extraction) 2 kilos potassium hydroxide KOH Bomb nickel coted 630 Grams red phosphorus 630 Grams yellow phosphorus (optional) 5250 Grams ethyl alcohol iodine 10500 grams iodine crystals 300 600 (synthesis) (super mercados) (synthesis) grams methanolic solution methylamine hydrochloride MeNH2•HCl grams sodium hydroxide NaOH .1000 ml.s 5400 6000 liquid ammonia (triethylamine and methylamine synthesis) (triethylamine and methylamine synthesis) (triethylamine and methylamine synthesis) (triethylamine and methylamine synthesis) (triethylamine and methylamine synthesis) (triethylamine and methylamine synthesis) (triethylamine and methylamine synthesis) (synthesis) (ethyl iodide synthesis) (ethyl iodide synthesis) (ethyl iodide synthesis) (ethyl iodide synthesis) (ethyl iodide synthesis) (solution) (chines) grams sodium hydroxide ml.s benzene triethylamine (synthesis) (lojas de tintas) (synthesis) (synthesis) 100 grams methylamine 10500 ml. as its boiling point is above room temperature vs. and then reaction with methylamine to form an alpha-hydroxy imine (1-Hydroxycyclopentyl-(ochlorophenyl)-ketone-N-methylimine). Both of these compounds are most likely more potent and longer lasting than ketamine. Overall yields are ~60%. Heating this imine results in Ketamine via a novel alpha-hydroxyimine rearangement (refs. The general necessity of producing anhydrous methylamine in a clandestine setting. 64). 20. 24 ). .Ketamine 200 grams methylketimine 2000 ml. Tiletamine is synthesized by an analogous process in industry. 22. and its N-ethyl analog. Two other ketamine analogs have been found on the black market: the compound missing the 2-chloro group on the phenyl ring. it is obtained exclusively by diversion of commercial sources rather than synthesis. Although it is currently a popular and common drug on the illicit market. 23. substituting 2-thiophenyl magnesium bromide for the phenyl grignard and ethylamine for methylamine. The syntheis starts with the reaction of cyclopentyl Grignard and o-chlorobenzonitrile to give o-chlorophenyl-cyclopentyl ketone. Synthesis of Ketamine (2) Ketamine is more difficult to synthesize than the previously considered PCP derivatives. increases the difficulty. followed by alpha bromination of the ketone. Use of propylamine rather than methylamine would simplify this reaction. with a difficulty rating of 2-3 out of 10 and a hazard rating of 1-2 out of 10 (ref.s undecane 20% hydrochloric acid HCl Dichloromethane DCM (solvent) Pentane / ether or hexane / ether (synthesis) (ver ) (solution) (lojas de tintas) (ver) …………………………………………………………………………………………………. rather than purchasing it. which is a gas at room temperature. This route has an overall yield of ~60%. 21. methylamine. 1 grams sulfuric acid HgSO4. collecting the fraction boiling at 128130°C. Dry with magnesium sulphate MgSO4. mp 118°C. The hot distillate is saturated with sodium chloride NaCl. Yield: 51 grams (89% of theory). ………………………………………………………………………………………………… Aluminium isopropoxide Al(i-PrO)3 .Synthetic procedure for ketamine synthesis: Step 1: (o-chlorophenyl)-cyclopentyl ketone Cyclopentanone 100 grams adipic acid and 10 grams Ba(OH)2 is intimately mixed and placed into a flask with a thermometer. .s in theory) abs. 70 ml. which lasts about 1-2 hrs. The rxn is heated to 280 °C.s (51ml. the mixture initially melts and then the distillation takes place. The mixture is heated. the upper layer is decanted and distilled.s RBF equipped with an efficient reflux condenser there's added 6 gams Al foil. Into a 250 ml.Bp 130-140°C at 7mmHg. isopropanol IPA (commercial reagent grade IPA was used without any drying) and 0. which causes acetone with some water to distill off. The obtained solution is immediately used as is in the following preparation ………………………………………………………………………………………………. Yield = 58 ramsg (74%) cyclopentyl Grignard reagent 119.s (50 grams ) cyclopentanone in 50 ml.00 a pound and is unwatched and uncontrolled.s Macrophage inflammatory protein-1β (MIP-1β) is a CC chemokine CCl4 (CAREFUL! Extremely toxic!) and heating continued until hydrogen gas H2 evolution starts. After the rxn subsides. The rxn is gently heated. …………………………………………………………………………………………………. which contains about 40 grams Al isopropoxide. The rxn is left for 24hrs with vigorous stirring.0 grams of cyclopentyl bromide and 19. Drying with magnesium sulphate MgSO4. The distillation is ended when the temp of the vapors rises to ~85°C. After that it’s diluted with 200 ml. collecting the fraction boiling at 137-140°C.s (45 grams) cyclopentanol and 60 ml. Distill. Yield: 47 grams (94%) ………………………………………………………………………………………………… Cyclopentyl bromide In a flask there’s mixed 47 ml. The ppt inside the flask is carefully decomposed with 50% sulfuric acid H2SO4 until acidic and saturated with sodium chloride NaCl. This stuff is 5% sodium hypochlorite. The upper layer is decanted and distilled. HBr. This stuff costs about US$5.ml. when it is stopped. Cyclopentanol Into a 250 ml. Now go to the chemicalsupply and get a pound or so of phthalimide. sometimes even cooling's needed. Yep. the same stuff as Clorox bleach but twice as strong and several times less expensive.5 .s (90 grams) 48% aq. Dryed with mangnesium sulphate MgSO4.In the beginning of boiling 0. 10 grams sodium sulphate Na2SO4 is added.4 grams of magnesium are reacted in ether or tetrahydrofuran THF to give a cyclopentyl Grignard reagent. but you have to wait for it to come in. Quantities can be purchased also in 25 pound bags. heating is continued until almost full dissolution of aluminium metal Al (5-7 hrs).s water and the lower organic phase is separated and washed with water twice. Phthalimide to anthranilic acid Go to the great big building supply house and pick up a couple of gallons of swimming pool chlorination liquid... collecting the fraction between 137-138°C. .s isopropanol IPA and the solT from the previous prep'n.s RBF equipped with a 15 cm Vigreux column and distilling condenser there's added 53 ml. It'll also try to crawl up the sides of the flask a half inch or so. Don't you just love it when people say. Be careful. Pour the boiling solution through 2 coffee filter using only gravity. Mix well and cool to less than 30 °C. This is about 4 rounded tablespoons for the scale impared out there. Discard the filtered yellow solution. the less the time. it is not very soluble in boiling water and almost not at all in cold water. Keep this put-powder-in-flask. The anthranillic acid forms long thin needle crystal that just love to attach to bubbles forming in the boiling water and foam up. After all the solutions (you'll have multiple containers) have cooled. The phthalimide will not dissolve. Now add 40 grams of phthalimide all at once. When the boiling solution starts to cool. but it will certainly turn dark and ruin the batch. The residual powder in the filter and flask needs another boiling water treatment to get some more anthranilic acid. The solution's temperature will rise and start to release gas. so it will take a heck of a lot of water to do the job. Some one may read how the solubility of the anthranillic in water can be increased by adding sodium hydroxide NaOH to the water. .s of destiled water and boil. add 300 ml. To clean this stuff dissolve it in boiling water. So filter quick and get the filter paper out and lay it on a couple of paper towels to wick away more of the solution. it will get wet and mix in the solution. add an equal volume of cold water. Just bring it to a boil and filter. This foam will easily boil out of the flack if you don't pay attention.s of destiled water. The anthranilic will try to cling to the sides of the flask and you'll have to rinse the flask a few times to get it all into the filter paper. Remember cooler is better) the reaction will happen. It would be best if you take it a half mile away just to be sure. You now have quite a pile of slightly impure anthranilic acid that needs to be recrystalized to purify. Stir this mess rapidly. When recrystalizing don't boil the solution too long or it will turn dark. It will appear to boil with the phthalimide changing into anthranilic acid and foaming on the top of the now yellow colored liquid.s of the hypochlorite solution and 400 ml. This is true. stir to cool down and vacuum filter to collect the solids.In a 2 liter erlinmeyer flask put 200 ml. more will form until at around 25 C° it's all out of solution. be sure to add the water to cool it off and filter it quickly to make sure the operation doesn't proceed to far. watching it for boil over. it will immediately crystalize into pretty white crystals. start off cool. Keep the sodium hydroxide NaOH in the cupboard on the other side of the room. filter and let the water cool to recrystalize the anthranilic. Heat is your enemy in the first part of the reaction. If it gets too hot it'l turn dark and clean up is horrible. This operation will take as much as 4 liters of water. 20 °C is a perfect temperature. "recrystalize from water. vacuum filter and dry the powder. As it cools off. After a couple of minutes of stirring (the warmer the solution. DO NOT try to dissolve all of it in the water. filter operation going until you don't get crystals in the filtered water. However. Possiblities of screw up. so be patient and keep with it. it will eat right through the filter if you take too long filtering it. Shake the flask and try to keep it all wet. One thing to note here is that you should use two coffee filters to filter this. boil. Do it like this: put the anthranilic in a 1 liter flask. Let the reaction proceed for 3 minutes shaking often. this is ok since it will also rinse away the rest of the bleach solution leaving slightly yellow crystals. This is concentrated anthranilic acid and bleach."? You try this and either nothing happens and you lose your product or it comes out dirtier than when you started. then do the next boiling operation. there isn't enough product in there to bother with. but it will also result in the anthranilic decomposing. you may be able to do it. Sodium bicarbonate Na2CO3... o-Bromobenzoic acid can bee obtained in an analogous manner. substituting copper chloride CuCl for CuBr CuBr …………………………………………………………………………………………………. A vigorous evolution of nitrogen is observed.The crystals when dry are mostly small needles.7 grams anthranilic acid is stirred in a glass beaker in 40 ml. The yield is only around 50%. the ppt is filtered. nitro. With constant stirring and cooling there's added 8 grams sodium nitrite NaNO2 in 40 ml. . but at US$5. of 10 grams copper chloride CuCl in 25 grams hydrochloric acid HCl conc.acids. that fluff up and take a lot of space for the weight.7 grams Hydrochloric acid HCl (conc. Needless to say there is substantial mechanical loss to this procedure.and oxy. 200 ml.19) 8 grams NaNO2 (sodium nitrite) 10 grams CuCl (Copper Chlorides) (synthesis) (chines) (synthesis) (ver where to get) 13.s 5% hypochlorite solution destiled water 40 grams phthalimide o-Chlorobenzoic acid Anthranilic acid 13.s hydrochloric acid HCl and 20 grams ice. and it can be a pain in the butt. o-chlorobenzonitrile Preparation A. but can bee used for bromo. This rxn is unsuitable for amino-.and chlorobenzoic acids.00 for the phthalimide and almost nothing for the sodium hypochlorite it is really cost effective and provides one with a good source of this controlled substance. When the rxn ends. Thus obtained clear solution of diazonium salt is very slowly added with stirring into a soln.s destiled water. (RCOO)2Zn + Pb(SCN)2 = 2 RCN + ZnS + PbS + 2 CO2 The best results are obtained when a zinc salt is employed instead of free acid. 28 ml. The product represents fine crystals and melts at 140-141°C. d=1.. washed with cold water and reprecipitated from aq.s 400 ml.s water. Sulfaminic acid is dirt cheap and can be acquired without causing any suspicion. then heated on open flame .1 mm Hg). C. bp 232°C. containing some ammonium hydroxide.1 mm Hg lead to some decomposition. steam-distilled and salted out. Distilled nitrile is treated with hydroxide ammonia NH4OH. Yield 137 grams (80%). The mixture is coffee ground and dried at 120-140°C for a prolonged time. The reaction is then hydrolyzed by pouring it onto a mixture of crushed ice and ammonium chloride. This bromoketone is unstable and must be used immediately.3 mm Hg) (CAS# 6740-85-8). Yield is ~66%. Step 2: alpha-bromo (o-chlorophenyl)-cyclopentyl ketone To 21. ……………………………………………………………………………………………. This is washed with a dilute aqueous solution of sodium bisulfite and evaporated to give 1-bromocyclopentyl-(o-chlorophenyl)-ketone. Preparation B.To a hot soln of 50 grams sodium hydroxide NaOH in 400 ml.s water there's added 195 grams o-chlorobenzoic acid. so it should be used without further purification.. bp 96-97 C (0.2 grams of o-chlorobenzonitrile is then added to the reaction mixture and stirred for three days. The bromination may also be carried out with N-bromosuccinimide in somewhat higher yields (~77%).s destiled water. The rxn usually takes place within 30-60 mins. bp 111-114 C (0. …………………………………………………………………………………………………. but the duration of dryings makes the method quite time-consuming. N-bromosuccinimide (NBS) .0 grams of bromine in 80 ml. such as benzene.s of carbon tetrachloride dropwise at 0 deg.0 grams of the above ketone is added 10. Also attempts to distill it at 0. mp 43-46°C. 55. The precipitated salt is dried for prolonged time at 200°C and mixed intimately with 205 grams Lead(II) thiocyanate Pb(SCN)2. The best yields are obtained if the ether solvent is distilled from the Grignard under vacuum and replaced with hydrocarbon solvent. Carefully neutralize with ammonia hydride NH3 or sodium bicarbonate NaHCO3 and add with heating 105 grams (~5% excess) zinc sulphate ZnSO4 in 400 ml.the mixture melts and gases are evolved. an orange suspension forms. After all of the Br2 has been added. This one doesn't require a prolonged drying. Extracion of the mixture with organic solvent gives o-chlorophenylcyclopentylketone. s (1. I think it's very time consuming and HCl is pretty nasty. Dry in a desiccator.60mol (64 grams) sodium hydroxide NaOH.s destiled water. not even a bit.65 mol. it doesn't hurt. Yield 75-81%. Only drawback with this method is that one must have good quality formaldehyde. Stir for two more minutes. If you do like said below.1.62 mol (160 grams) succinimide 1. 264 grams) Br2 Methylamine from Ammonium Chloride and Formaldehyde Many bees are making methylamine out of hexamine and HCl acid. Don't clean up NBS too much. 300 grams crushed ice 400 ml.60mol (64 grams) sodium hydroxide NaOH. and add 85 ml. the stinky yellow stuff still containing a bit of Br2 works best. you get around 400-450 grams of pretty pure dimethylamine-free methylamine hydrochloride which is perfect for Al/Hg reductive aminations. 264 grams) Br2 at once while stirring violently. Thus I have found that one can easily make lots of good quality methylamine from ammonium chloride and formaldehyde (formalin).s destiled water 85 ml. It may have paraformaldehyde sediment in the bottom.62 mol (160 grams) succinimide is dissolved in a mixture of 1.65 mol. 1.s (1. Now to the more-less foolproof method. then filter the precipitated product and wash with ice water. 300 grams crushed ice and 400 ml. but Formaldehyde has to be strong and not some diluted shit. Cool the mixture in an ice bath. 35-40% is fine. Chemicals needed: • • • 1100g of Ammonium Chloride 2 liters of 35-40% Formaldehyde about half a litre of chloroform The process . [ At 40°C ] . an exothermic reaction kicks in (it needs to be cooled in a water bath once in a while at the beginning in order to keep temperature below 104-106°C). I used a 12 L RB flask.Pour your formaldehyde in a big round bottom flask (use at least one of 5 liter capacity) along with ammonium chloride and stir a bit.[At 80°C] At about 90°C. Start heating slowly. and stir it every once in a while. . Soon reaction slows down and cooling isn't needed anymore. reaction flask must be heated carefully to keep temperature at 104-106°C. Keep that temperature 3-4 hours or so. then turn heat up and boil water away until you see ammonium chloride coming out of solution. Cool to 20°C and . Transfer it to a smaller flask and boil water away until you see the internal temperature rise over 160°C. first temperature falls a few tens of degrees and when it rises back to about 160°C the methylamine is almost free of water. then turn on the vacuum and continue.vacuum filter it off on large Buchner funnel (I have one with Ø 25 cm). Turn off the vacuum and the heat. You should get a clear yellowish filtrate like in this picture. . you can still see some orange liquid at the bottom of the beaker).Pour your crude methylamine hydrochloride in a beaker. . At first it is still liquid (in this picture it has started to solidify. .HCl picks up water from air like nothing. You can only use vacuum for sucessful drying but these CHCl3 traces don't hurt the methylamine at all and may be left in. you'll have a big chunk of hard and dry methylamine... The smell can be removed by drying in a vacuum desiccator.When it has cooled down.HCl which reeks of chloroform. Vacuum filter to get pure and dry Methylamine. Do not try to use the oven to get rid of these traces of chloroform. but you might perhaps be a perfectionist. the Methylamine. Wash it a few times with chloroform and you'll end up with a fully white mush. ... and the resulting acidic solution is made basic.. has a mp of 92-93C.. The residue is then dissolved in pentane and filtered....Final yield of snow white non-sticky powder....... easily exceeds 400g if everything done correctly........... (consisting of methylamine with a few percent ammonium chloride...s of decalin and refluxed for 2... The solvent is evaporated to yield 1hydroxy-cyclopentyl-(o-chlorophenyl)-ketone N-methylimine......... 2.... but and almost no dimethylamine hydrochloride)..... The hydrochloride has a mp of 262-263 C..0 grams of above bromoketone is dissolved in 50 ml.... ... the residue is extracted with dilute hydrochloric acid. after recrystallization from pentane-ether. mp 62 C (yield ~84%)... 2-methylamino-2-(ochlorophenyl)-cyclohexanone (Ketamine). Benzene may also be used as solvent................ and gives almost quantitative yield after 180 C for 30 min....... After one hour.............. Step 4: 2-Methylamino-2-(o-chlorophenyl)-cyclohexanone (Ketamine) The final step is a thermal rearrangement......... or even 500g if you used 40% formaldehyde.. the excess liquid methylamine is allowed to evaporate.....0 grams of the preceeding N-methylimine is dissolved in 15 ml..5 h. An alternative to the use of decalin as solvent in this step is to use a pressure bomb. the solution treated with decolorizing charcoal............................s of liquid methylamine freebase....... although increasing the reaction time to 4-5 days may increase yield....... The liberated product. ........ Step 3: 1-hydroxycyclopentyl-(o-chlorophenyl)-ketone-N-methylimine 29. After evaporation of the solvent under reduced pressure..... farmacias) (conservar e restaurar) grams HgSO4 (sulfuric acid) ml.s 123 620 isopropanol IPA (super market) (conservar e restaurar . farmacias) (synthesis) .As with PCE.ls 6120 grams IPA isopropanol Al isopropoxide (synthesis) ( conservar e restaurar . ………………………………………………………………………………………………… Total synthesis 100 grams Step 1: (o-chlorophenyl)-cyclopentyl ketone Cyclopentanone 17000 grams adipic acid 1700 grams Ba(OH)2 (Barium hydroxide ) Sodium chloride NaCl (table salt) MgSO4 ( magnesium sulphate) ( ver) ( ebay) (super market) (farmacias) Aluminium isopropoxide 7344 grams Al foil 85680 ml.s (7650g) cyclopentanone 7650 m.s CCl4(Macrophage inflammatory protein-1β (MIP-1β) is a CC chemokine ) (ver) Cyclopentanol 8109 ml. and must be converted into the hydrochloric HCl salt in order to be consumed in this manner. the freebase is too caustic to be smoked. s o-Chlorobenzoic acid 15228 152400 304800 30480 grams Anthranilic acid ml.cyclopentyl bromide 5355 grams cyclopentanol (synthesis) ( synthesis) 10710 grams 48% aq.s ml.s grams 5% hypochlorite solution destiled water phthalimide (synthesis) (anthranilic acid synthesis)(lojas de piscinas) (anthranilic acid synthesis) (anthranilic acid synthesis) (ebay ver) (chines) ( synthesis) Hydrochloric acid HCl (conc. HBr (hydrobromic acid) 220g KBr (potassium bromide) or 190g NaBr (sodium bromide)((hydrobromic acid synthesis) 200 ml.s concentrated H2SO4 (hydrobromic acid synthesis) (hydrobromic acid synthesis) ( by product hydrobromic acid synthesis) grams Na2SO4 sodium sulphate destiled water Sodium chloride NaCl (table salt ) 50% sulfuric acid H2SO4 MgSO4 magnesium sulphate (synthesis) (synthesis) (super market) (solution) (farmacias) K2SO4 1190 23800 ml..s distilled water 90 ml. d=1.19) 8736 grams NaNO2 ( sodium nitrite) 6804 GRAMS NITRIC ACID HNO3 (NaNO2 sodium nitrite) 6724 GRAMS SODIUM CARBONATE (SODA ASH) (NaNO2 sodium nitrite) 10920 grams CuCl (Copper Chlorides) 12 kilos copper wire (synthesis) ( Copper Chlorides synthesis) . s 10920 grams o-chlorobenzoic acid NH3 ammonia hydroxide or NaHCO3 (sodium bicarbonate) (chines / super market) 5880 grams (~5% excess) ZnSO4 (zinc sulphate) 11480 grams Pb(SCN)2 (Lead(II) thiocyanate) NH4OH (hydroxide de amonio) (ver) (ver synthesis) cyclopentyl Grignard reagent (synthesis) 11900 grams cyclopentyl bromide 1940 grams magnesium turnings ether or thf benzene (opitional) 5520 grams o-chlorobenzonitrile ammonium chloride 1 LITRO ACIDO CLORIDRICO 1 LITRO DE AMONIACO ammonium hydroxide (synthesis) (where to get) (synthesis) (lojas de tintas) (synthesis) (synthesis) (Ammonium chloride synthesis) (Ammonium chloride synthesis) (chines e farmacias) .(ver) CuCO3 20 % hydrochloric acid HCl solution ( Copper Chlorides synthesis) ( Copper Chlorides synthesis) o-chlorobenzonitrile 1800 grams sodium hydroxide NaOH destiled water (chines) (synthesis) (synthesis) 44800 ml. 60mol (64 grams) sodium hydroxide NaOH 300 grams crushed ice 400 ml.s methylamine (synthesis) (synthesis) (methylamine synthesis) (methylamine synthesis) (methylamine synthesis) 14300 grams Ammonium Chloride 26 6500 liters 35-40% Formaldehyde ml.62 mol (160 grams) succinimide 1.s carbon tetrachloride sodium bisulfite N-bromosuccinimide (OPITIONAL) 1. 264 grams) Br2 (synthesis) (lojas de piscinas e ebay) (where to buy) (ebay) (synthesis) (N-bromosuccinimide synthesis) (N-bromosuccinimide synthesis) (N-bromosuccinimide synthesis) (N-bromosuccinimide synthesis) (N-bromosuccinimide synthesis) Step 3: 1-hydroxycyclopentyl-(o-chlorophenyl)-ketone-N-methylimine 2900 grams alpha-bromo (o-chlorophenyl)-cyclopentyl ketone 5000 ml.s destiled water 85 ml.Step 2: alpha-bromo (o-chlorophenyl)-cyclopentyl ketone 2100 grams o-chlorophenyl)-cyclopentyl ketone 1000 grams bromine 8000 ml.65 mol.s (1.s chloroform 14300 LITRO ACIDO CLORIDRICO 14300 LITRO DE AMONIACO Benzene (opitional) pentane ? (Ammonium chloride synthesis) (Ammonium chloride synthesis) (lojas de tintas) (ver) . s 200 decalin (solvent) (OPITIONAL) (ver) (synthesis) (chines) (ver) (ver) grams 1-hydroxycyclopentyl-(o-chlorophenyl)-ketone-N-methylimine hydrochloric acid decolorizing charcoal pentane-ether .Step 4: 2-Methylamino-2-(o-chlorophenyl)-cyclohexanone (Ketamine) 1500 ml.