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All 7 posts Subject: Perposed peptide coupling (LSD) Please login to post Down

MakoEyes
(Stranger)
11-13-04 14:33
No 541377
      Perposed peptide coupling (LSD)

ok heres what SWIM is thinking of for a LSD synth

1) A/B extraction of HBWR seeds (850g).    yeild: 2.5g misc ergot alkaloids
2) Hydrolysis of extracted Ergot alkaloids.    yeild: 1g Lysergic Acid
3) Distilation of DEET to Diethylamine.    yeild: 2g Diethylamine
4) Coupling of LSA with Diethylamine via PyBOP. yeild: 1.7g D-Lysergic Acid Diethylamine

step 1
A/B extraction of HBWR seeds (850g).
1) Wash/dry seeds... Powder 850g of seeds in a clean blender or coffie grinder. Air dry the resulting powder.
2) Submerge podwer in VM&P Naptha (petrolium ether) in a flask, stopper flask, shake vigorusly, let sit for 2 days in a dark place shaking every once in a while.
3) Vacume filter, save/dry resulting mush (dry in vacuo).
4) Submerge powder in ahydronus MeOH in a flask, stoper flask let sit 2 days in a dark place shaking every once in a while.
5) Vacume filter, save the MeOH this time. Revome solovent in vacuo.

step 2
Hydrolysis of extracted Ergot alkaloids.
1) Dissolve 2.5g of the alkaloid in 22 ml of 1 M methanolic KOH solution (this is made by dissolving 1.4 g of KOH in 25 ml of dry methanol).
2) In a 1 1iter evaporation flask (heavy walled construction) immediately Evaporate the methanol off.
3) Add 40 ml of 8% aqueous (water) KOH solution to the residue and boil for one hour under a slow stream of nitrogen that is allowed to flow through a small orifice for exhausting purposes.
4) Cool, acidify with dilute sulfuric acid, and shake in a separatory funnel with 1 1iter of dry ether. Separate the lower aqueous layer .
5) Vacuum filter. Wash the precipitate with 2 ml of dilute sulfuric acid. This is lysergic acid.

step 3
distilation of DEET to Diethylamine.
1) Mix DEET with an excess of 10-20% aqueous NaOH.
2) Distill, collect the distillate in dilute HCl.
3) Evaporate HCl to get Diethylamine Hydrochloride.

step 4
Coupling of LSA with Diethylamine via PyBOP.
1) Dissolve 1g LSA in ahydronus Toluene at RT.
2) Add 1.05 g PyBOP.
3) Add 2g of diethylamine stir reaction at RT until it goes to completion (15min-2hr).
4) Remove the Toluene under vacuum.
5) Partition the residue between EtOAc (or other suitable solvent) and saturated NaHCO3 (or NH4OH).
6) Wash the organics with NaHCO3 (or NH4OH) and H2O.
7) Saturate with NaCl.
8) Dry over MgSO4.
9) Filter and concentrate in vacuo to remove the solvent and excess diethylamine.
10) Converte to the tartrate salt.

any thoughts? Will the Hydrolysis work in this somewhat smaller scale?

$800 for ~15000 hits of acid? dont mind if i do.(humor, ya know a joke)

"He who makes a beast of himself gets rid of the pain of being a man" Dr. Johnson

Lilienthal
(Moderator)
11-13-04 15:51
No 541384
User Picture       You have omitted the hard part on every stage.

You have omitted the hard part on every stage. The purification steps are what makes this chemistry so difficult, column chromatography is mandatory. And of course it is NOT possible to use methanol as a solvent in the coupling reaction. Before starting to calculate fake yields and your profit you have to acquire a lot laboratory practice with more simple or with small scale reactions under TLC control.

MakoEyes
(Stranger)
11-13-04 17:11
No 541389
      "You have omitted the hard part on every...

"You have omitted the hard part on every stage."
such as?, chromotography yes, im looking at a lover grade here, do you think it possable to run a column at the end of the synth?

indole_amine
(Hive Bee)
11-13-04 17:48
No 541395
User Picture       chromatography and other purification steps...

You left out almost every thinkable purification step so far; and this is the reason why it won't work.

_{indole_amine}

MakoEyes
(Stranger)
11-13-04 18:09
No 541400
      ic

what would you reccomend as a modification of this procedure? is there any way to use non-chromotography purification methods? as far as purity goes is my main concern the purification of my ergot alkaliods or is it my post hydrolized LSA? what adulterants am i looking to eliminate? once agian thank you for any help.

MakoEyes
(Stranger)
11-13-04 18:21
No 541402
      oh yeah

i was also wondering if said impurities made this synth impossable or just dirty i do remember noodle claiming to have yeilded LSD from non-chromatographed percursors. i guess what im after is how foriving will each reaction be and what ratios of regants can i use to perhapse make a reaction more forgiving, i realize by nature an lsd synth is pretty goddamned rigid; but is a peptide coupling more forgiving than previous methods?

indole_amine
(Hive Bee)
11-13-04 18:35
No 541404
User Picture       let me try to explain

Ok. You at least agree that a final purification step is necessary; do you? crazy So let's apply a simple mathematic rule of the theory of probability - saying that when repeatedly throwing one dice, the probability for a certain combination of several numbers (like 4/3/6/1/2) is 1 / X^n with n = number of throws and X being the number of possibilities for each throw (or a probability of n = 1 / 6^5 for [4/3/6/1/2] in that order). And with every throw, the probability for every combination gets smaller by the factor X^ⁿ⁺¹ or in other words: the probability diminishes exponentially with every further throw.

Transcribed to your idea of running only one final column, this would mean that with each non-purified precursor or pre-precursor, you could as well throw dices to determine the success of rxn: because in both cases, the probability for a clean end product (or right combination of [success/success/success] with X=2, n=3 and therefore n=1 / 2^³ = 12.5% probability for overall success after three "dirty" rxns wink ) gets diminished drastically if you don't influence the probability for "success" at each stage through purification, and with a multiple-step synthesis like the one you described, this means a very low probability for a successful end reaction and clean end product, or maybe a very small probability for the case that the final column is sufficient if you want so... smile

And believe me, it's nice to be able to correctly predict the results before attempting synths with reagents worth >800 bucks (not counting the many hours of dirty lab work) - and unpredictable results at this stage of investments are not cool; and you can believe me here too frown ...

_{indole_amine}

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	All 7 posts		Subject: Perposed peptide coupling (LSD)		Please login to post		Down


		MakoEyes (Stranger) 11-13-04 14:33 No 541377				Perposed peptide coupling (LSD)
						ok heres what SWIM is thinking of for a LSD synth 1) A/B extraction of HBWR seeds (850g). yeild: 2.5g misc ergot alkaloids 2) Hydrolysis of extracted Ergot alkaloids. yeild: 1g Lysergic Acid 3) Distilation of DEET to Diethylamine. yeild: 2g Diethylamine 4) Coupling of LSA with Diethylamine via PyBOP. yeild: 1.7g D-Lysergic Acid Diethylamine step 1 A/B extraction of HBWR seeds (850g). 1) Wash/dry seeds... Powder 850g of seeds in a clean blender or coffie grinder. Air dry the resulting powder. 2) Submerge podwer in VM&P Naptha (petrolium ether) in a flask, stopper flask, shake vigorusly, let sit for 2 days in a dark place shaking every once in a while. 3) Vacume filter, save/dry resulting mush (dry in vacuo). 4) Submerge powder in ahydronus MeOH in a flask, stoper flask let sit 2 days in a dark place shaking every once in a while. 5) Vacume filter, save the MeOH this time. Revome solovent in vacuo. step 2 Hydrolysis of extracted Ergot alkaloids. 1) Dissolve 2.5g of the alkaloid in 22 ml of 1 M methanolic KOH solution (this is made by dissolving 1.4 g of KOH in 25 ml of dry methanol). 2) In a 1 1iter evaporation flask (heavy walled construction) immediately Evaporate the methanol off. 3) Add 40 ml of 8% aqueous (water) KOH solution to the residue and boil for one hour under a slow stream of nitrogen that is allowed to flow through a small orifice for exhausting purposes. 4) Cool, acidify with dilute sulfuric acid, and shake in a separatory funnel with 1 1iter of dry ether. Separate the lower aqueous layer . 5) Vacuum filter. Wash the precipitate with 2 ml of dilute sulfuric acid. This is lysergic acid. step 3 distilation of DEET to Diethylamine. 1) Mix DEET with an excess of 10-20% aqueous NaOH. 2) Distill, collect the distillate in dilute HCl. 3) Evaporate HCl to get Diethylamine Hydrochloride. step 4 Coupling of LSA with Diethylamine via PyBOP. 1) Dissolve 1g LSA in ahydronus Toluene at RT. 2) Add 1.05 g PyBOP. 3) Add 2g of diethylamine stir reaction at RT until it goes to completion (15min-2hr). 4) Remove the Toluene under vacuum. 5) Partition the residue between EtOAc (or other suitable solvent) and saturated NaHCO3 (or NH4OH). 6) Wash the organics with NaHCO3 (or NH4OH) and H2O. 7) Saturate with NaCl. 8) Dry over MgSO4. 9) Filter and concentrate in vacuo to remove the solvent and excess diethylamine. 10) Converte to the tartrate salt. any thoughts? Will the Hydrolysis work in this somewhat smaller scale? $800 for ~15000 hits of acid? dont mind if i do.(humor, ya know a joke) "He who makes a beast of himself gets rid of the pain of being a man" Dr. Johnson



		Lilienthal (Moderator) 11-13-04 15:51 No 541384				You have omitted the hard part on every stage.
						You have omitted the hard part on every stage. The purification steps are what makes this chemistry so difficult, column chromatography is mandatory. And of course it is NOT possible to use methanol as a solvent in the coupling reaction. Before starting to calculate fake yields and your profit you have to acquire a lot laboratory practice with more simple or with small scale reactions under TLC control.



		MakoEyes (Stranger) 11-13-04 17:11 No 541389				"You have omitted the hard part on every...
						"You have omitted the hard part on every stage." such as?, chromotography yes, im looking at a lover grade here, do you think it possable to run a column at the end of the synth?



		indole_amine (Hive Bee) 11-13-04 17:48 No 541395				chromatography and other purification steps...
						You left out almost every thinkable purification step so far; and this is the reason why it won't work. _{indole_amine}



		MakoEyes (Stranger) 11-13-04 18:09 No 541400				ic
						what would you reccomend as a modification of this procedure? is there any way to use non-chromotography purification methods? as far as purity goes is my main concern the purification of my ergot alkaliods or is it my post hydrolized LSA? what adulterants am i looking to eliminate? once agian thank you for any help.



		MakoEyes (Stranger) 11-13-04 18:21 No 541402				oh yeah
						i was also wondering if said impurities made this synth impossable or just dirty i do remember noodle claiming to have yeilded LSD from non-chromatographed percursors. i guess what im after is how foriving will each reaction be and what ratios of regants can i use to perhapse make a reaction more forgiving, i realize by nature an lsd synth is pretty goddamned rigid; but is a peptide coupling more forgiving than previous methods?



		indole_amine (Hive Bee) 11-13-04 18:35 No 541404				let me try to explain
						Ok. You at least agree that a final purification step is necessary; do you? So let's apply a simple mathematic rule of the theory of probability - saying that when repeatedly throwing one dice, the probability for a certain combination of several numbers (like 4/3/6/1/2) is 1 / X^n with n = number of throws and X being the number of possibilities for each throw (or a probability of n = 1 / 6^5 for [4/3/6/1/2] in that order). And with every throw, the probability for every combination gets smaller by the factor X^ⁿ⁺¹ or in other words: the probability diminishes exponentially with every further throw. Transcribed to your idea of running only one final column, this would mean that with each non-purified precursor or pre-precursor, you could as well throw dices to determine the success of rxn: because in both cases, the probability for a clean end product (or right combination of [success/success/success] with X=2, n=3 and therefore n=1 / 2^³ = 12.5% probability for overall success after three "dirty" rxns ) gets diminished drastically if you don't influence the probability for "success" at each stage through purification, and with a multiple-step synthesis like the one you described, this means a very low probability for a successful end reaction and clean end product, or maybe a very small probability for the case that the final column is sufficient if you want so... And believe me, it's nice to be able to correctly predict the results before attempting synths with reagents worth >800 bucks (not counting the many hours of dirty lab work) - and unpredictable results at this stage of investments are not cool; and you can believe me here too ... _{indole_amine}

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