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	Tryptamine Chemistry

All 9 posts Subject: Neophyte Chemist's Questions On Synthesis of LSD Please login to post Down

Hierofant
(Stranger)
10-27-03 23:17
No 467121
      Neophyte Chemist's Questions On Synthesis of LSD

Using the second procedure of LSD synthesis from the book "Psycadelic Guide to the Preparation of the Eucharist"(Will be quoted in a following post) how necessary is it to perform the chemical reactions in a nitrogen or vacuum environment? If it is completely necessary without damaging the yield incredibly which would be better to use a nitrogen or vacuum environment? Is it necessary to clean the Lysergic Acid with ether? Will there be any toxic chemicals with the Lysergic Acid if not cleaned with ether? Thanks for any help you can give.

Hierofant
(Stranger)
10-27-03 23:20
No 467122
      from "Psychedelic Guide to the ...

from "Psychedelic Guide to the Preparation of the Eucharist" by Robert Brown, 1967.

--------------------------------------------------------------------------------

Preparatory arrangements:
Starting material may be any lysergic acid derivative, from ergot on rye grain or from culture, or morning glory seeds or from synthetic sources. Preparation #1 uses any amide, or lysergic acid as starting material. Preparations #2 and #3 must start with lysergic acid only, prepared from the amides as follows:

10 g of any lysergic acid amide from various natural sources dissolved in 200 ml of methanolic KOH solution and the methanol removed immediately in vacuo. The residue is treated with 200 ml of an 8% aqueous solution of KOH and the mixture heated on a steam bath for one hour. A stream of nitrogen gas is passed through the flask during heating and the evolved NH3 gas may be titrated is HCl to follow the reaction. The alkaline solution is made neutral to congo red with tartaric acid, filtered, cleaned by extraction with ether, the aqueous solution filtered and evaporated. Digest with MeOH to remove some of the coloured material from the crystals of lysergic acid.

Arrange the lighting in the lab similarly to that of a dark room. Use photographic red and yellow safety lights, as lysergic acid derivatives are decomposed when light is present. Rubber gloves must be worn due to the highly poisonous nature of ergot alkaloids. A hair drier, or, better, a flash evaporator, is necessary to speed up steps where evaporation is necessary.

Preparation #2

Step I. Use Yellow light
5.36 g of d-lysergic acid are suspended in 125 ml of acetonitrile and the suspension cooled to about -20 C in a bath of acetone cooled with dry ice. To the suspension is added a cold (-20 C) solution of 8.82 g of trifluoroacetic anhydride in 75 ml of acetonitrile. The mixture is allowed to stand at -20 C for about 1.5 hours during which the suspended material dissolves, and the d-lysergic acid is converted to the mixed anhydride of lysergic and trifluoroacetic acids. The mixed anhydride can be separated in the form of an oil by evaporating the solvent in vacuo at a temperature below 0 C, but this is not necessary. Everything must be kept anhydrous.

Step II. Use Yellow light
The solution of mixed anhydrides in acetonitrile from Step I is added to 150 ml of a second solution of acetonitrile containing 7.6 g of diethylamine. The mixture is held in the dark at room temperature for about 2 hours. The acetonitrile is evaporated in vacuo, leaving a residue of LSD-25 plus other impurities. The residue is dissolved in 150 ml of chloroform and 20 ml of ice water. The chloroform layer is removed and the aqueous layer is extracted with several portions of chloroform. The chloroform portions are combined and in turn washed with four 50 ml portions of ice-cold water. The chloroform solution is then dried over anhydrous Na2SO4 and evaporated in vacuo.

Oxygen
(Stranger)
10-28-03 02:36
No 467177
      inert gas, etc

I think it is better to be safe than sorry with the inert gas when working with lysergic acid--meaning that all of the reactions should be done in inert gas and in the dark. Any toxic chemicals present would be present in the final product in only very tiny amounts per dose, but if you don't eliminate the impurities then you could throw off your ratios and have difficulty measuring yields.

Acetonitrile and trifluoroacetic anhydride are easier to get than POCl₃. US Patent 2,736,728 describes the process: https://www.rhodium.ws/chemistry/lsdpatent.html (about halfway down the page). I would think that they are less suspicious too. I wonder if it would be safe to use lysergic acid monohydrate instead of dry lysergic acid by adding an extra molar equivalent of trifluoroacetic anhydride.

Next on the list - ditrifluoroacetylmorphine. tongue

doktor_alternate
(Newbee)
05-09-04 07:25
No 505954
      seems that d-tartaric acid is very expensive...

seems that d-tartaric acid is very expensive (some $230 for each 50g or so) this could be a special biochemical preparation (s*gma*****ch.com), but as it stands, this would be one of the more expensive reagents in the formation of LSD tartrate. shulgin seems to like it alot... but are there any other salts (maleate or something) that are significantly less expensive?

doktor_alternate
(Newbee)
05-10-04 01:55
No 506113
      the key here is that

the d-tartrate salt of lsd is reportedly stable indefinately. which other salts would achieve this? hydrobromide? citric? ascorbic? (this would scavenge free radicals too)

ning
(acetaminophanatic)
05-10-04 14:03
No 506213
User Picture       I'm no expert on acid

but a little bee told me that:

1. Cream of tartar in the supermarket is sodium tartrate. Think about that. Funny, isn't it?

2. I think they use tartaric acid as part of the chiral resolution process, as well. It is chiral as well. The natural product is non-racemic. See point <1> above.

3. I heard a little bit of ascorbic acid helps the shelf life of acid.

I'm going to have to call UTFSE on this one now, since you now know the keywords to search.

Lastly, I'll hint that diethylamine, always a handy thing to have when discussing acid, could bee made by hydrolyzing DEET, the bug repellent. Search for that too.

Wink wink nudge nudge.

-ning

_{...it's an AOL chatroom for dyslexic spider monkies...}

Rhodium
(Chief Bee)
05-10-04 16:32
No 506241
User Picture       chirality of otc tartrate salts

"Cream of tartar" consists of potassium hydrogen tartrate, not sodium tartrate. "Rochelle salt" is potasium sodium tartrate.

The supermarket tartaric acid salts can be based on either synthetic (racemate) or the natural L-tartaric acid depending on country/location/brand, but never the more expensive synthetic D-tartaric acid, which unfortunately is the form which crystallizes best with LSD.

^{The Hive - Clandestine Chemists Without Borders}

ning
(acetaminophanatic)
05-11-04 16:12
No 506456
User Picture       Ah well

It seems I have been corrected laugh

Rodium, what do you think about the use of ascorbic acid? If it crystallized well, it would probably have desireable antioxidant properties.

_{...it's an AOL chatroom for dyslexic spider monkies...}

timnickbear
(Stranger)
05-12-04 21:45
No 506723
      LSD maleate

I believe that the emetic activities of lysergamides by johnson et al in the 70's lists the use of maleate rather than tartrate because tartrate seems to oxydise whereas maleate doesnt

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	All 9 posts		Subject: Neophyte Chemist's Questions On Synthesis of LSD		Please login to post		Down


		Hierofant (Stranger) 10-27-03 23:17 No 467121				Neophyte Chemist's Questions On Synthesis of LSD
						Using the second procedure of LSD synthesis from the book "Psycadelic Guide to the Preparation of the Eucharist"(Will be quoted in a following post) how necessary is it to perform the chemical reactions in a nitrogen or vacuum environment? If it is completely necessary without damaging the yield incredibly which would be better to use a nitrogen or vacuum environment? Is it necessary to clean the Lysergic Acid with ether? Will there be any toxic chemicals with the Lysergic Acid if not cleaned with ether? Thanks for any help you can give.



		Hierofant (Stranger) 10-27-03 23:20 No 467122				from "Psychedelic Guide to the ...
						from "Psychedelic Guide to the Preparation of the Eucharist" by Robert Brown, 1967. -------------------------------------------------------------------------------- Preparatory arrangements: Starting material may be any lysergic acid derivative, from ergot on rye grain or from culture, or morning glory seeds or from synthetic sources. Preparation #1 uses any amide, or lysergic acid as starting material. Preparations #2 and #3 must start with lysergic acid only, prepared from the amides as follows: 10 g of any lysergic acid amide from various natural sources dissolved in 200 ml of methanolic KOH solution and the methanol removed immediately in vacuo. The residue is treated with 200 ml of an 8% aqueous solution of KOH and the mixture heated on a steam bath for one hour. A stream of nitrogen gas is passed through the flask during heating and the evolved NH3 gas may be titrated is HCl to follow the reaction. The alkaline solution is made neutral to congo red with tartaric acid, filtered, cleaned by extraction with ether, the aqueous solution filtered and evaporated. Digest with MeOH to remove some of the coloured material from the crystals of lysergic acid. Arrange the lighting in the lab similarly to that of a dark room. Use photographic red and yellow safety lights, as lysergic acid derivatives are decomposed when light is present. Rubber gloves must be worn due to the highly poisonous nature of ergot alkaloids. A hair drier, or, better, a flash evaporator, is necessary to speed up steps where evaporation is necessary. Preparation #2 Step I. Use Yellow light 5.36 g of d-lysergic acid are suspended in 125 ml of acetonitrile and the suspension cooled to about -20 C in a bath of acetone cooled with dry ice. To the suspension is added a cold (-20 C) solution of 8.82 g of trifluoroacetic anhydride in 75 ml of acetonitrile. The mixture is allowed to stand at -20 C for about 1.5 hours during which the suspended material dissolves, and the d-lysergic acid is converted to the mixed anhydride of lysergic and trifluoroacetic acids. The mixed anhydride can be separated in the form of an oil by evaporating the solvent in vacuo at a temperature below 0 C, but this is not necessary. Everything must be kept anhydrous. Step II. Use Yellow light The solution of mixed anhydrides in acetonitrile from Step I is added to 150 ml of a second solution of acetonitrile containing 7.6 g of diethylamine. The mixture is held in the dark at room temperature for about 2 hours. The acetonitrile is evaporated in vacuo, leaving a residue of LSD-25 plus other impurities. The residue is dissolved in 150 ml of chloroform and 20 ml of ice water. The chloroform layer is removed and the aqueous layer is extracted with several portions of chloroform. The chloroform portions are combined and in turn washed with four 50 ml portions of ice-cold water. The chloroform solution is then dried over anhydrous Na2SO4 and evaporated in vacuo.



		Oxygen (Stranger) 10-28-03 02:36 No 467177				inert gas, etc
						I think it is better to be safe than sorry with the inert gas when working with lysergic acid--meaning that all of the reactions should be done in inert gas and in the dark. Any toxic chemicals present would be present in the final product in only very tiny amounts per dose, but if you don't eliminate the impurities then you could throw off your ratios and have difficulty measuring yields. Acetonitrile and trifluoroacetic anhydride are easier to get than POCl₃. US Patent 2,736,728 describes the process: https://www.rhodium.ws/chemistry/lsdpatent.html (about halfway down the page). I would think that they are less suspicious too. I wonder if it would be safe to use lysergic acid monohydrate instead of dry lysergic acid by adding an extra molar equivalent of trifluoroacetic anhydride. Next on the list - ditrifluoroacetylmorphine.



		doktor_alternate (Newbee) 05-09-04 07:25 No 505954				seems that d-tartaric acid is very expensive...
						seems that d-tartaric acid is very expensive (some $230 for each 50g or so) this could be a special biochemical preparation (sgma****ch.com), but as it stands, this would be one of the more expensive reagents in the formation of LSD tartrate. shulgin seems to like it alot... but are there any other salts (maleate or something) that are significantly less expensive?



		doktor_alternate (Newbee) 05-10-04 01:55 No 506113				the key here is that
						the d-tartrate salt of lsd is reportedly stable indefinately. which other salts would achieve this? hydrobromide? citric? ascorbic? (this would scavenge free radicals too)



		ning (acetaminophanatic) 05-10-04 14:03 No 506213				I'm no expert on acid
						but a little bee told me that: 1. Cream of tartar in the supermarket is sodium tartrate. Think about that. Funny, isn't it? 2. I think they use tartaric acid as part of the chiral resolution process, as well. It is chiral as well. The natural product is non-racemic. See point <1> above. 3. I heard a little bit of ascorbic acid helps the shelf life of acid. I'm going to have to call UTFSE on this one now, since you now know the keywords to search. Lastly, I'll hint that diethylamine, always a handy thing to have when discussing acid, could bee made by hydrolyzing DEET, the bug repellent. Search for that too. Wink wink nudge nudge. -ning _{...it's an AOL chatroom for dyslexic spider monkies...}



		Rhodium (Chief Bee) 05-10-04 16:32 No 506241				chirality of otc tartrate salts
						"Cream of tartar" consists of potassium hydrogen tartrate, not sodium tartrate. "Rochelle salt" is potasium sodium tartrate. The supermarket tartaric acid salts can be based on either synthetic (racemate) or the natural L-tartaric acid depending on country/location/brand, but never the more expensive synthetic D-tartaric acid, which unfortunately is the form which crystallizes best with LSD. ^{The Hive - Clandestine Chemists Without Borders}



		ning (acetaminophanatic) 05-11-04 16:12 No 506456				Ah well
						It seems I have been corrected Rodium, what do you think about the use of ascorbic acid? If it crystallized well, it would probably have desireable antioxidant properties. _{...it's an AOL chatroom for dyslexic spider monkies...}



		timnickbear (Stranger) 05-12-04 21:45 No 506723				LSD maleate
						I believe that the emetic activities of lysergamides by johnson et al in the 70's lists the use of maleate rather than tartrate because tartrate seems to oxydise whereas maleate doesnt

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