Finshaggy
Well-Known Member
I am not suggesting that anyone use this information, it is just too God damn simple not to share with everyone. I am not saying it is easy stuff that anyone can do (the MDA one is, the DMT one is not), I am saying it is not hard to figure out and extremely obvious and in our faces.
MDMA is great right? But it's hard to make, so what if you could just mix 3 things together, and put it in your freezer, and expect ecstasy to form? Well now you can. (It's like Sham Wow, except I am not going to start boxing hookers after I share this with you)
MDA is a VERY close relative to MDMA, in fact you need to make MDA in order to make MDMA... And some people say they like MDA MORE than MDMA, because of MDMA's methylated Amphetamine molecule, it has a speedier effect while MDA is more sensory (Read Erowid for more specific discrepancies).
According to popular alkaloidal synthesis procedure:
15 Grams of Piperonal in 80ml Glacial Acetic Acid + 15ml Nitroethane + 10g Cyclohexylamine, This combination is heated with a boiling water bath for 6 hours, removed from the heat and diluted with 10ml of distilled water and left in a cold ice bath. Yellow crystals should precipitate and should be filtered and allowed to dry. This is MDA.
DMT is simply an altered and Di methylated Tryptophan molecule. YES, the same stuff that makes you sleepy on Thanks Giving is the structural back bone of DMT. Here is how you make DMT with Tryptophan found in Milk (From Rhodium)
L-Tryptophan From Milk
Casein[SUP]6[/SUP]
To 1 liter of milk, from which the cream has been largely separated (by simple skimming), 0.05 M hydrochloric acid is slowly added, with stirring through a capillary tube extending to the bottom of the beaker. The addition is continued until the solution attains a pH of 4.6 (casein exists in milk in the form of a calcium derivative; pH 4.6 is the isoelectric point of free casein, which is soluble to the extent of only 0.11g/L water). Approximately 1 L of acid is required; the separation of the casein is practically complete at this point. Three liters of water is then added, stirring is discontinued, and the flocculent precipitate of casein is allowed to settle in the refrigerator for twelve to twenty-four hours. The clear supernatant liquid which contains soluble proteins and salts is removed as completely as possible by siphoning; the precipitate is collected on a suction funnel and washed with cold distilled water until the washings are free of calcium (test with ammonium oxalate)The casein, which is contaminated with calcium phosphate and fats; is filtered to as small a volume as possible (about 500 mL) and transferred to a 2000ml beaker. It is then treated with 0.1 M sodium hydroxide, the alkali being added slowly and with stirring through a capillary extending to the bottom of the beaker (it is important to avoid a local excess of alkali, which would tend to denaturate the casein). The addition of alkali is continued until the pH of the mixture reaches 6.3 (at this pH sodium caseinate is largely dissolved, whereas calcium caseinate is largely undissolved); 100-150 mL of the alkali is required. At this pH the casein is completely in solution in the form of its sodium salt; fats, calcium phosphate, and any calcium caseinate remain undissolved. Care must be taken not to add more alkali than is necessary to bring the pH to the above point. The milky solution is filtered through a thick layer (10-15 mm.) of filter paper pulp tightly packed upon a suction funnel. The filtrate may be slightly opalescent; if it is less clear it is again filtered through a fresh layer of pulp.The filtrate is brought to a pH of 4.6 with 0.05 M hydrochloric acid just as in the original precipitation, the necessary amount of acid being determined by titration of an aliquot portion, diluted fivefold, with 0.01 M hydrochloric acid, 220-250 mL of 0.05 M acid is required. As the reprecipitation progresses, the rate at which the acid is added is decreased in order to prevent precipitation at the tip of the capillary tube; vigorous mechanical stirring is, of course, essential. When the acidification is complete, 5000ml of cold distilled water is added and the flocculent precipitate allowed to settle in the refrigerator. After siphoning off the clear supernatant liquid, the casein is collected on a suction funnel, using hardened paper, washed with cold distilled water until free of chloride, sucked as dry as possible, and dried over calcium chloride in a vacuum desiccator. The yield is 23-29 g. of a colorless coherent product which may readily be pulverized in a mortar.
To a solution of L-tryptophan (50g) in water was added a solution of an excess of copper(II)acetate in water. The resultant precipitate was filtered. The extract was then washed several times with hot water to give the copper chelate compound. Yield: 52g, mp >280°C.
[h=5]L-Tryptophan[SUP]7[/SUP][/h]In an 8 Liter bottle is placed 600g of commercial casein (coarse powder), which is then covered with about 3200 mL of tap water at 37°C. The bottle is shaken until all the casein is moistened. A solution of 60 g. of anhydrous sodium carbonate and 6 g. of sodium fluoride (to inhibit oxidase enzymes present) in 1 L of water at 37°C is added. A thin paste of 20 g. of commercial pancreatin in 100 mL of water (37°C) is poured in. The mixture is covered with a layer of toluene (80 mL), diluted to 6 L, stoppered, shaken thoroughly, and placed in a warm room or bath at 37°C. After four or five days, with daily shakings, most of the casein is in solution and chalky masses of tyrosine begin to separate. After five days, a second 20-g. portion of pancreatin in 100 mL of water is added. After twelve days, the bottle is cooled in an icebox overnight and the undissolved material is filtered off (This filtration may be slow. Büchner funnels of 20-cm. diameter are best used; the material from a single filling is allowed to suck dry and the filter paper then changed).The filtrate (6.9-7 L) is measured into a 16-L stone jar, and for every liter there is added 163 mL of dilute sulfuric acid (one volume of 95 per cent sulfuric acid and one volume of water, cooled to room temperature). The first part of the acid must be added cautiously on account of the liberation of carbon dioxide. The tryptophan is precipitated by adding a solution of 200 g. of mercuric sulfate (Note 5) in a mixture of 1860 mL of water and 140 mL of 95 per cent sulfuric acid. After standing for twenty-four to fortyeight hours, the clear liquid is siphoned out and the yellow precipitate is filtered and washed with a solution of 100 mL of concentrated sulfuric acid in 1.9 L of distilled water containing 20 g. of mercuric sulfate, until the filtrate is colorless and Millon's test is atypical; about 1.5 L is necessary. The precipitate is washed with three successive 500-mL portions of distilled water to remove most of the sulfuric acid.The moist precipitate (120-130 g) is suspended with mechanical stirring in 1.2-1.3 L of distilled water, and a hot, 20 per cent aqueous solution of barium hydroxide is added until the mixture is permanently alkaline to phenolphthalein (about 120 mL is required). A rapid stream of hydrogen sulfide is passed in with stirring until the mercury is completely precipitated. The precipitate is filtered and washed with water until a sample of the washings gives a negative test for tryptophan with bromine water. The barium is removed from the combined filtrate and washings by adding the exact amount of dilute sulfuric acid and filtering. The filtrate is concentrated under reduced pressure to about 80 mL.The tryptophan is extracted from the aqueous solution by repeated shaking in a separatory funnel with 25-mL quantities of n-butyl alcohol; water is added from time to time to keep the volume approximately constant. The butyl alcohol extract is distilled under reduced pressure. After the water present has distilled, the tryptophan precipitates in the distilling flask and may cause bumping. When all the water has been removed, as is indicated by non-formation of drops on the side of the condenser, the distillation is stopped and, after cooling, the tryptophan is filtered and washed with a little fresh butyl alcohol. Such extractions and distillations are continued until the quantities of tryptophan obtained are negligibly small.The tryptophan so produced (7-8 g.) varies somewhat in quality in different runs. It is purified by recrystallization from 60 mL of dilute alcohol (two volumes of 95% alcohol to one volume of water), filtering from the hot solution an appreciable quantity of insoluble matter, and subjecting this to a second extraction with an additional 10 mL of aqueous alcohol. The solution is decolorized by the addition of 1 g. of Norite and allowed to stand in the icebox; the silvery leaflets of tryptophan are filtered and washed successively with cold 70 per cent, 80 per cent, 95% alcohol, and, finally, with a little ether. Less than half the tryptophan is obtained in each crystallization. The yield of pure tryptophan is 4.0-4.1 g., together with under 0.1 g of less pure product.
Decarboxylation of the Tryptophan Copper Chelate
A suspension of Tryptophan Copper Chelate in DMSO was heated at 170-175°C for several minutes, during which time an evolution of carbon dioxide was observed. After cooling, the resultant precipitate was filtered and to the filtrate was added a suitable amount of water. The reaction mixture was made basic with 30% sodium hydroxide solution and extracted with chloroform. After distillation of the solvent, the resultant residue was purified by flash chromatography on silica gel to givce tryptamine in 40% yield. The use of HMPA (hexamethylphosphoric triamide) instead of DMSO increased the yield to 45%, but that small increase in yield is not worth working with the expensive and highly toxic solvent HMPA.
OR
A mixture of 75 mL of turpentine (1), 7.14 grams of L-tryptophan (2), and 15 drops (0.25 grams; 0.3 mL) of spearmint oil (3) were placed in a 250 mL Erlenmeyer flask. A water cooled reflux condenser(4) was attached to the flask by a rubber stopper (5). The mixture in the flask was boiled (6)fast enough that there was at least one drop returning to the flask from the condenser every second. The mixture became transparent in four hours and heating was turned off after another 30 minutes. There was a little yellow solid on the side of the flask above the liquid. After sitting overnight there was a clump of yellow crystals in the corner of the flask and solidified dark oil across the bottom. The flask was refrigerated for the day and the orangish mother liquor was poured off.The impure tryptamine was purified as follows (7). To the flask were added 150 mL of 5% distilled household vinegar along with 5 mL of chloroform (
and the flask was briskly swirled until all solid was gone and there was only a little dark brown oil not dissolved in the yellow suspension. The hazy yellow liquid (pH 5-6) upper layer was filtered through a plug of cotton. The small amount of dark brown lower organic layer was extracted with another 10 mL of vinegar, and the resulting upper layer was filtered through the cotton plug. To the combined filtrates were added 5 mL of chloroform and enough sodium bicarbonate (10.58 g) in portions so that further addition caused very little foaming. The flask was swirled thoroughly and the hazy yellow aqueous upper layer was filtered through a fresh plug of cotton. The filtrate was cooled in the freezer for 15 minutes, basified with 12 mL of 25% sodium hydroxide solution, and set back in the freezer for 30 minutes. The solid was dislodged from the sides with a metal scoop and the mixture was filtered through filter paper (9). The flask and crystals were rinsed with 100 mL of ice cold household ammonia in portions (10). The filter paper was pressed between paper towels until damp and set aside to dry. The light yellow crystals weighed 3.64 grams (65% yield).The turpentine mother liquor from the last reaction, still containing spearmint oil and some tryptamine, was used directly to decarboxylate 7.23 grams of L-tryptophan. This time the reaction took seven hours to become transparent, so apparently some of the catalyst was consumed during the first reaction. This time both the turpentine and the solid product were extracted with vinegar as above, and brought through the same purification process, to give 5.21 grams (92% yield) of light yellow crystals. The combined yield of tryptamine for the last two reactions is 79%. The solid melted at 117-118.5°C (Merck 118°C) and had one tan spot (R[SUB]f[/SUB] ~0.1 - 0.2) on silica TLC, eluting with methanol containing ~50 mg of ammonium carbonate.
And this point you can either make DMT or AMT (or a variety of other things)
DMT
Next, 30g of formaldehyde and 120g Tryptamine were disolved in 1800ml of MeOH, to this was slowly added dropwise 50g of NaCNBH[SUB]3[/SUB] disolved in 550ml MeOH. Then 14g Glacial Acetic Acid was added dropwise with stirring. The mixture was then stirred for 60 hours. The majority of the MeOH was distilled off (2000 ml collected) to the distillation flask was added 1L of 5% Aq. Ammonia which was extracted with 3x250ml of DCM. The DCM was washed with a salt solution (not saturated but still pretty strong) then the DCM separated and dried with a large portion of anhydrous MgSO[SUB]4[/SUB]. The DCM was distilled off at atmospheric pressure and then the distillation was continued under vacuum (~1 torr now) until the dimethyltryptamine was collected. Which was recrystalized from boiling hexane with a few mls of Ethyl Acetate added. This afforded 48.8g of DMT, a 35% yield.
AMT
Enantiomerically pure alpha-methyltryptamine can be made through reduction of the ethyl esters of D- and L-tryptophan, respectively. (+)-AMT is approximately four times as potent a CNS stimulant as (-)-AMT.
R(+)-2-Amino-3-(3-indolyl)propanol
One g. (3.58 mmoles) of D-tryptophan ethyl ester hydrochloride was added in portions to a stirred suspension of 800 mg (21 mmoles) of lithium aluminum hydride in 15 ml. of dry tetrahydrofuran at room temperature. After stirring for 30 minutes, the complex was decomposed by dropwise addition of 2N sodium hydroxide. The solids were filtered and shaken with 50 ml. of 2N sodium hydroxide and 200 ml. of chloroform in a separatory funnel. The organic layer was separated, combined with the original filtrate and dried (magnesium sulfate). The drying agent was removed by filtration and the filtrate concentrated at reduced pressure. The syrupy residue was crystallized from ethyl acetate/ hexane, yield 450 mg (66%).
R(+)-N-(Benzyloxycarbonyl)-2-amino-3-(3-indolyl)-propanol
R(+)-2-Amino-3-(3-indolyl)propanol (1.32 g., 6.95 mmoles) was dissolved in a mixture of 30 ml. of water and 30 ml. of acetone. Sodium carbonate (1.27 g., 12 mmoles) was added and to the stirred, cooled mixture (ice) was added dropwise 1.0 ml. (7.0 mmoles) of benzyl chloroformate. After the addition the cooling bath was removed and the reaction stirred at room temperature for 1.5 hours. The reaction mixture was acidified (to pH 2) with concentrated hydrochloric acid and diluted with 100 ml. of water. The aqueous mixture was extracted with 2x150 ml of ethyl acetate, the organic solution washed with 100 ml. of saturated aqueous sodium chloride and dried (magnesium sulfate). Filtration of the drying agent and concentration in vacuo left a syrupy residue which was crystallized from chloroform/hexane to give 1.7 g. (75%).
R(+)-N-(Benzyloxycarbonyl)-2-amino-3-(3-indolyl)propanol p-Toluenesulfonate
R(+)-N-(Benzyloxycarbonyl)-2-amino-3-(3-indolyl)-propanol (350 mg., 1.08 mmoles) was dissolved in 10 ml. of dry pyridine and 310 mg (1.62 mmoles) of p-toluenesulfonyl chloride was added. The reaction was stored at room temperature for 18 hours and the solvent distilled under reduced pressure. The residue was partitioned between 200 ml of ethyl acetate and 50 ml. of saturated aqueous sodium chloride. The organic layer was washed with 50 ml. of water and dried (magnesium sulfate). Filtration and concentration in vacuo left a foamy residue. Pure product was isolated by preparative TLC using 10% acetone in benzene, yield 400 mg (77%). This compound was unstable at room temperature but could be stored for several weeks at -15°C.
S(+)-3-(2-Aminopropyl)indole p-Toluenesulfonate
R(+)-N-(Benzyloxycarbonyl)-2-amino-3-(3-indolyl)propanol p-Toluenesulfonate (400 mg., 0.84 mmole) was dissolved in 25 mL of absolute ethanol and 100 mg. of 10% palladium on charcoal catalyst added. The reaction mixture was shaken under 3 atmospheres of hydrogen for one hour. The catalyst was filtered (Celite) and the filtrate concentrated under reduced pressure. The residual oil was taken up in 6 ml. of hot chloroform and cooled to room temperature. The precipitate was filtered and dried in vacuo. It was recrystallized from methanol/ether, yield 240 mg (82%).
S(+)-3-(2-Aminopropyl)-indole (S(+)-alpha-methyl-tryptamine)
S(+)-3-(2-Aminopropyl)indole p-Toluenesulfonate (100 mg., 0.289 mmole) was stirred in 10 ml. Of 2N sodium hydroxide for 5 minutes. The oily product was extracted with 2x50 ml. of ethyl acetate and the organic solution was dried (magnesium sulfate), filtered and concentrated under reduced pressure. The syrupy residue was crystallized from ethyl acetate/hexane, yield 35 mg. (69%).
MDMA is great right? But it's hard to make, so what if you could just mix 3 things together, and put it in your freezer, and expect ecstasy to form? Well now you can. (It's like Sham Wow, except I am not going to start boxing hookers after I share this with you)
MDA is a VERY close relative to MDMA, in fact you need to make MDA in order to make MDMA... And some people say they like MDA MORE than MDMA, because of MDMA's methylated Amphetamine molecule, it has a speedier effect while MDA is more sensory (Read Erowid for more specific discrepancies).
According to popular alkaloidal synthesis procedure:
15 Grams of Piperonal in 80ml Glacial Acetic Acid + 15ml Nitroethane + 10g Cyclohexylamine, This combination is heated with a boiling water bath for 6 hours, removed from the heat and diluted with 10ml of distilled water and left in a cold ice bath. Yellow crystals should precipitate and should be filtered and allowed to dry. This is MDA.
DMT is simply an altered and Di methylated Tryptophan molecule. YES, the same stuff that makes you sleepy on Thanks Giving is the structural back bone of DMT. Here is how you make DMT with Tryptophan found in Milk (From Rhodium)
L-Tryptophan From Milk
Casein[SUP]6[/SUP]
To 1 liter of milk, from which the cream has been largely separated (by simple skimming), 0.05 M hydrochloric acid is slowly added, with stirring through a capillary tube extending to the bottom of the beaker. The addition is continued until the solution attains a pH of 4.6 (casein exists in milk in the form of a calcium derivative; pH 4.6 is the isoelectric point of free casein, which is soluble to the extent of only 0.11g/L water). Approximately 1 L of acid is required; the separation of the casein is practically complete at this point. Three liters of water is then added, stirring is discontinued, and the flocculent precipitate of casein is allowed to settle in the refrigerator for twelve to twenty-four hours. The clear supernatant liquid which contains soluble proteins and salts is removed as completely as possible by siphoning; the precipitate is collected on a suction funnel and washed with cold distilled water until the washings are free of calcium (test with ammonium oxalate)The casein, which is contaminated with calcium phosphate and fats; is filtered to as small a volume as possible (about 500 mL) and transferred to a 2000ml beaker. It is then treated with 0.1 M sodium hydroxide, the alkali being added slowly and with stirring through a capillary extending to the bottom of the beaker (it is important to avoid a local excess of alkali, which would tend to denaturate the casein). The addition of alkali is continued until the pH of the mixture reaches 6.3 (at this pH sodium caseinate is largely dissolved, whereas calcium caseinate is largely undissolved); 100-150 mL of the alkali is required. At this pH the casein is completely in solution in the form of its sodium salt; fats, calcium phosphate, and any calcium caseinate remain undissolved. Care must be taken not to add more alkali than is necessary to bring the pH to the above point. The milky solution is filtered through a thick layer (10-15 mm.) of filter paper pulp tightly packed upon a suction funnel. The filtrate may be slightly opalescent; if it is less clear it is again filtered through a fresh layer of pulp.The filtrate is brought to a pH of 4.6 with 0.05 M hydrochloric acid just as in the original precipitation, the necessary amount of acid being determined by titration of an aliquot portion, diluted fivefold, with 0.01 M hydrochloric acid, 220-250 mL of 0.05 M acid is required. As the reprecipitation progresses, the rate at which the acid is added is decreased in order to prevent precipitation at the tip of the capillary tube; vigorous mechanical stirring is, of course, essential. When the acidification is complete, 5000ml of cold distilled water is added and the flocculent precipitate allowed to settle in the refrigerator. After siphoning off the clear supernatant liquid, the casein is collected on a suction funnel, using hardened paper, washed with cold distilled water until free of chloride, sucked as dry as possible, and dried over calcium chloride in a vacuum desiccator. The yield is 23-29 g. of a colorless coherent product which may readily be pulverized in a mortar.
To a solution of L-tryptophan (50g) in water was added a solution of an excess of copper(II)acetate in water. The resultant precipitate was filtered. The extract was then washed several times with hot water to give the copper chelate compound. Yield: 52g, mp >280°C.
[h=5]L-Tryptophan[SUP]7[/SUP][/h]In an 8 Liter bottle is placed 600g of commercial casein (coarse powder), which is then covered with about 3200 mL of tap water at 37°C. The bottle is shaken until all the casein is moistened. A solution of 60 g. of anhydrous sodium carbonate and 6 g. of sodium fluoride (to inhibit oxidase enzymes present) in 1 L of water at 37°C is added. A thin paste of 20 g. of commercial pancreatin in 100 mL of water (37°C) is poured in. The mixture is covered with a layer of toluene (80 mL), diluted to 6 L, stoppered, shaken thoroughly, and placed in a warm room or bath at 37°C. After four or five days, with daily shakings, most of the casein is in solution and chalky masses of tyrosine begin to separate. After five days, a second 20-g. portion of pancreatin in 100 mL of water is added. After twelve days, the bottle is cooled in an icebox overnight and the undissolved material is filtered off (This filtration may be slow. Büchner funnels of 20-cm. diameter are best used; the material from a single filling is allowed to suck dry and the filter paper then changed).The filtrate (6.9-7 L) is measured into a 16-L stone jar, and for every liter there is added 163 mL of dilute sulfuric acid (one volume of 95 per cent sulfuric acid and one volume of water, cooled to room temperature). The first part of the acid must be added cautiously on account of the liberation of carbon dioxide. The tryptophan is precipitated by adding a solution of 200 g. of mercuric sulfate (Note 5) in a mixture of 1860 mL of water and 140 mL of 95 per cent sulfuric acid. After standing for twenty-four to fortyeight hours, the clear liquid is siphoned out and the yellow precipitate is filtered and washed with a solution of 100 mL of concentrated sulfuric acid in 1.9 L of distilled water containing 20 g. of mercuric sulfate, until the filtrate is colorless and Millon's test is atypical; about 1.5 L is necessary. The precipitate is washed with three successive 500-mL portions of distilled water to remove most of the sulfuric acid.The moist precipitate (120-130 g) is suspended with mechanical stirring in 1.2-1.3 L of distilled water, and a hot, 20 per cent aqueous solution of barium hydroxide is added until the mixture is permanently alkaline to phenolphthalein (about 120 mL is required). A rapid stream of hydrogen sulfide is passed in with stirring until the mercury is completely precipitated. The precipitate is filtered and washed with water until a sample of the washings gives a negative test for tryptophan with bromine water. The barium is removed from the combined filtrate and washings by adding the exact amount of dilute sulfuric acid and filtering. The filtrate is concentrated under reduced pressure to about 80 mL.The tryptophan is extracted from the aqueous solution by repeated shaking in a separatory funnel with 25-mL quantities of n-butyl alcohol; water is added from time to time to keep the volume approximately constant. The butyl alcohol extract is distilled under reduced pressure. After the water present has distilled, the tryptophan precipitates in the distilling flask and may cause bumping. When all the water has been removed, as is indicated by non-formation of drops on the side of the condenser, the distillation is stopped and, after cooling, the tryptophan is filtered and washed with a little fresh butyl alcohol. Such extractions and distillations are continued until the quantities of tryptophan obtained are negligibly small.The tryptophan so produced (7-8 g.) varies somewhat in quality in different runs. It is purified by recrystallization from 60 mL of dilute alcohol (two volumes of 95% alcohol to one volume of water), filtering from the hot solution an appreciable quantity of insoluble matter, and subjecting this to a second extraction with an additional 10 mL of aqueous alcohol. The solution is decolorized by the addition of 1 g. of Norite and allowed to stand in the icebox; the silvery leaflets of tryptophan are filtered and washed successively with cold 70 per cent, 80 per cent, 95% alcohol, and, finally, with a little ether. Less than half the tryptophan is obtained in each crystallization. The yield of pure tryptophan is 4.0-4.1 g., together with under 0.1 g of less pure product.
Decarboxylation of the Tryptophan Copper Chelate
A suspension of Tryptophan Copper Chelate in DMSO was heated at 170-175°C for several minutes, during which time an evolution of carbon dioxide was observed. After cooling, the resultant precipitate was filtered and to the filtrate was added a suitable amount of water. The reaction mixture was made basic with 30% sodium hydroxide solution and extracted with chloroform. After distillation of the solvent, the resultant residue was purified by flash chromatography on silica gel to givce tryptamine in 40% yield. The use of HMPA (hexamethylphosphoric triamide) instead of DMSO increased the yield to 45%, but that small increase in yield is not worth working with the expensive and highly toxic solvent HMPA.
OR
A mixture of 75 mL of turpentine (1), 7.14 grams of L-tryptophan (2), and 15 drops (0.25 grams; 0.3 mL) of spearmint oil (3) were placed in a 250 mL Erlenmeyer flask. A water cooled reflux condenser(4) was attached to the flask by a rubber stopper (5). The mixture in the flask was boiled (6)fast enough that there was at least one drop returning to the flask from the condenser every second. The mixture became transparent in four hours and heating was turned off after another 30 minutes. There was a little yellow solid on the side of the flask above the liquid. After sitting overnight there was a clump of yellow crystals in the corner of the flask and solidified dark oil across the bottom. The flask was refrigerated for the day and the orangish mother liquor was poured off.The impure tryptamine was purified as follows (7). To the flask were added 150 mL of 5% distilled household vinegar along with 5 mL of chloroform (
and the flask was briskly swirled until all solid was gone and there was only a little dark brown oil not dissolved in the yellow suspension. The hazy yellow liquid (pH 5-6) upper layer was filtered through a plug of cotton. The small amount of dark brown lower organic layer was extracted with another 10 mL of vinegar, and the resulting upper layer was filtered through the cotton plug. To the combined filtrates were added 5 mL of chloroform and enough sodium bicarbonate (10.58 g) in portions so that further addition caused very little foaming. The flask was swirled thoroughly and the hazy yellow aqueous upper layer was filtered through a fresh plug of cotton. The filtrate was cooled in the freezer for 15 minutes, basified with 12 mL of 25% sodium hydroxide solution, and set back in the freezer for 30 minutes. The solid was dislodged from the sides with a metal scoop and the mixture was filtered through filter paper (9). The flask and crystals were rinsed with 100 mL of ice cold household ammonia in portions (10). The filter paper was pressed between paper towels until damp and set aside to dry. The light yellow crystals weighed 3.64 grams (65% yield).The turpentine mother liquor from the last reaction, still containing spearmint oil and some tryptamine, was used directly to decarboxylate 7.23 grams of L-tryptophan. This time the reaction took seven hours to become transparent, so apparently some of the catalyst was consumed during the first reaction. This time both the turpentine and the solid product were extracted with vinegar as above, and brought through the same purification process, to give 5.21 grams (92% yield) of light yellow crystals. The combined yield of tryptamine for the last two reactions is 79%. The solid melted at 117-118.5°C (Merck 118°C) and had one tan spot (R[SUB]f[/SUB] ~0.1 - 0.2) on silica TLC, eluting with methanol containing ~50 mg of ammonium carbonate.And this point you can either make DMT or AMT (or a variety of other things)
DMT
Next, 30g of formaldehyde and 120g Tryptamine were disolved in 1800ml of MeOH, to this was slowly added dropwise 50g of NaCNBH[SUB]3[/SUB] disolved in 550ml MeOH. Then 14g Glacial Acetic Acid was added dropwise with stirring. The mixture was then stirred for 60 hours. The majority of the MeOH was distilled off (2000 ml collected) to the distillation flask was added 1L of 5% Aq. Ammonia which was extracted with 3x250ml of DCM. The DCM was washed with a salt solution (not saturated but still pretty strong) then the DCM separated and dried with a large portion of anhydrous MgSO[SUB]4[/SUB]. The DCM was distilled off at atmospheric pressure and then the distillation was continued under vacuum (~1 torr now) until the dimethyltryptamine was collected. Which was recrystalized from boiling hexane with a few mls of Ethyl Acetate added. This afforded 48.8g of DMT, a 35% yield.
AMT
Enantiomerically pure alpha-methyltryptamine can be made through reduction of the ethyl esters of D- and L-tryptophan, respectively. (+)-AMT is approximately four times as potent a CNS stimulant as (-)-AMT.
R(+)-2-Amino-3-(3-indolyl)propanol
One g. (3.58 mmoles) of D-tryptophan ethyl ester hydrochloride was added in portions to a stirred suspension of 800 mg (21 mmoles) of lithium aluminum hydride in 15 ml. of dry tetrahydrofuran at room temperature. After stirring for 30 minutes, the complex was decomposed by dropwise addition of 2N sodium hydroxide. The solids were filtered and shaken with 50 ml. of 2N sodium hydroxide and 200 ml. of chloroform in a separatory funnel. The organic layer was separated, combined with the original filtrate and dried (magnesium sulfate). The drying agent was removed by filtration and the filtrate concentrated at reduced pressure. The syrupy residue was crystallized from ethyl acetate/ hexane, yield 450 mg (66%).
R(+)-N-(Benzyloxycarbonyl)-2-amino-3-(3-indolyl)-propanol
R(+)-2-Amino-3-(3-indolyl)propanol (1.32 g., 6.95 mmoles) was dissolved in a mixture of 30 ml. of water and 30 ml. of acetone. Sodium carbonate (1.27 g., 12 mmoles) was added and to the stirred, cooled mixture (ice) was added dropwise 1.0 ml. (7.0 mmoles) of benzyl chloroformate. After the addition the cooling bath was removed and the reaction stirred at room temperature for 1.5 hours. The reaction mixture was acidified (to pH 2) with concentrated hydrochloric acid and diluted with 100 ml. of water. The aqueous mixture was extracted with 2x150 ml of ethyl acetate, the organic solution washed with 100 ml. of saturated aqueous sodium chloride and dried (magnesium sulfate). Filtration of the drying agent and concentration in vacuo left a syrupy residue which was crystallized from chloroform/hexane to give 1.7 g. (75%).
R(+)-N-(Benzyloxycarbonyl)-2-amino-3-(3-indolyl)propanol p-Toluenesulfonate
R(+)-N-(Benzyloxycarbonyl)-2-amino-3-(3-indolyl)-propanol (350 mg., 1.08 mmoles) was dissolved in 10 ml. of dry pyridine and 310 mg (1.62 mmoles) of p-toluenesulfonyl chloride was added. The reaction was stored at room temperature for 18 hours and the solvent distilled under reduced pressure. The residue was partitioned between 200 ml of ethyl acetate and 50 ml. of saturated aqueous sodium chloride. The organic layer was washed with 50 ml. of water and dried (magnesium sulfate). Filtration and concentration in vacuo left a foamy residue. Pure product was isolated by preparative TLC using 10% acetone in benzene, yield 400 mg (77%). This compound was unstable at room temperature but could be stored for several weeks at -15°C.
S(+)-3-(2-Aminopropyl)indole p-Toluenesulfonate
R(+)-N-(Benzyloxycarbonyl)-2-amino-3-(3-indolyl)propanol p-Toluenesulfonate (400 mg., 0.84 mmole) was dissolved in 25 mL of absolute ethanol and 100 mg. of 10% palladium on charcoal catalyst added. The reaction mixture was shaken under 3 atmospheres of hydrogen for one hour. The catalyst was filtered (Celite) and the filtrate concentrated under reduced pressure. The residual oil was taken up in 6 ml. of hot chloroform and cooled to room temperature. The precipitate was filtered and dried in vacuo. It was recrystallized from methanol/ether, yield 240 mg (82%).
S(+)-3-(2-Aminopropyl)-indole (S(+)-alpha-methyl-tryptamine)
S(+)-3-(2-Aminopropyl)indole p-Toluenesulfonate (100 mg., 0.289 mmole) was stirred in 10 ml. Of 2N sodium hydroxide for 5 minutes. The oily product was extracted with 2x50 ml. of ethyl acetate and the organic solution was dried (magnesium sulfate), filtered and concentrated under reduced pressure. The syrupy residue was crystallized from ethyl acetate/hexane, yield 35 mg. (69%).
. Procedure:
