Author Topic: trouble getting yields for LSD  (Read 16462 times)

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montanha

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trouble getting yields for LSD
« on: February 25, 2002, 04:46:00 PM »
Guys, I have a few questions, and I guess some of you chemical killers can help me out.
First, I am trying to hydrolyse ergot tartrate that is 100% white, and in KOH solution continues white. I have a pharmacopeia that says ergotamine can be either white or yellow.
I am guessing the yellow one shulgin and everyone else mentions is the "other" type of ergotamine. What I want to ask is: has anyone ever worked w/ white ET? does it continue white in KOH solution? What I notice is that it turns yellow  ( maybe greenish-yellow ) under UV flashes.

Well, I purify my product and I usually get a little over what I'm supposed to ( maybe 10% in average) which I find strange.

Then I proceed to the POCL3 method, I heat up, add everything, and voilá. I dry my solvent after washing and when I dissolve in methanol, I  see that not EVERYTHING is dissolved. Then I add the maleic acid (20% in methanol) and very little crystalyzes. I don't get needles, but some sparse dust and I figure it's not even worth filtering.
I don;t plan to give up yet, so I dillute this whole thing in water, estimating that I have something like one gram of good LSD. I take it and I trip some. I give it to friends, and they say it's mild, but clean and the feeling is very pleasant.
My conclusion is: I DID get lsd, but why is it not crystalysing? I would like to remind that my lab is completely dark w/ blackout curtains, 20 square meters big w/ a 30000 BTU air conditioner and an extra dehumidifier, all My solvents(methanol and chloroform are HPLC, and I have an oven in which I dry all my glassware before use.
My reflux column is about -8C cold and a generous nitrogen flow (and bubbling) is present at all times in my reactions.

I have thermostats for my oil baths, the only thing I am guessing is not 100% is my vacuum pump, its giving me something like 30-40mm vacuum. Could this be so important?
I am waiting 2-3 days for drying solvents. Also, when I dry the LSD freebase, I don't get crystals, I get some sort of a plate, feels hard, but definitely is not a bunch of crystals.

Guys, help me out. I need to get some reasonable yield here.
(Oh, the ET source is pretty reliable) (and I DID get a very strong trip once, when I licked my instruments)

thanks for the time and knowledge

hest

  • Guest
Re: trouble getting yields for LSD
« Reply #1 on: February 25, 2002, 05:49:00 PM »
White is good, yellow is not so good, the collor comes from impurities. More informations thanks.
Let the malec acid/LSD solution stand in the fredge for a day ore too.
Iff you can get hold on some lyserg-something (amide,acid..) then you are home, the synthesis is not the problem. POCl3 is an 'unstabel' liquid, destilate it before use (just use a roto vap. thats fine)
You are the first person here to repoprt on an actual acid dream. If it's true you deserve a big congratulation.

montanha

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Re: trouble getting yields for LSD
« Reply #2 on: February 25, 2002, 08:34:00 PM »
I hope I understood something here: Im the only one tripping on my own acid? I don't believe so. What do you mean exactly by acid dream?
Also, I have a roto vap, but is it necessary to distill the POCL3? I have trouble imagining its fucked up. Ti decomposes w/ time or something? is there ways to avoid decomposition, and what are the co-products. I guess a good strategy would be to hydrolyze a lot of LSA and then distill a lot of POCL3, because to distill 2 ml at a time will cause a lot of waste, and this is not so easy to get.

Once it's distilled, for how long it's good for, considering it's in the dark, cold and dry?

Thanks a lot for your answer I never looked at the POCl3 as a possible problem.  ;)

Rhodium

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Re: trouble getting yields for LSD
« Reply #3 on: February 25, 2002, 08:44:00 PM »
Noone here at the Hive have written about any attempts to make LSD, ever. There are people with the knowledge, but without the needed chemicals or analytic equipment, and on the other hand there are the clueless people who believe that a synthesis of LSD is not considerably harder to pull off than one of MDMA or meth, and claim both here and there that they have made acid, when it is obvious that they don't even know what an epimerization is, or how they planned to avoid such a thing happening with their product, and how to purify the d-Lysergic acid diethylamide tartrate from epimers and decomposition products (for possible recycling).

bujinkan

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Re: trouble getting yields for LSD
« Reply #4 on: February 25, 2002, 11:40:00 PM »
montanha is truly a groundbreaker. So, based on your trip, what was your final estimation of yeild? can you tell us a little about your lighting setup?
heres to firsts at the hive.


oh, youasked "what is an acid dream?"
around here we dont actually carry out syntheses, we only dream of doing so. catch my drift?

Vibrating_Lights

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Re: trouble getting yields for LSD
« Reply #5 on: February 26, 2002, 12:50:00 AM »

Lilienthal

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Re: trouble getting yields for LSD
« Reply #6 on: February 26, 2002, 04:08:00 AM »
As long as you don't give experimental details like volumes / concentrations / reagents and so on, we can't help you. But here are some more general remarks.

There's only one type of ergotamine. Brown colors are forming in most organic syntheses and stem from minor byproducts. Usually you don't have to care about them as long as the substance is pure enough for your needs.

You don't need dim conditions if you are working with lysergamides. I posted a paper (->TFSE) with experiments showing that light is not that harmful to LSD as always thought. They used extremly diluted solutions, if you are handling gram quantities it shouldn't matter at all...

HPLC grade does not mean anhydrous. HPLC grade solvents may have a lot of water in them and have to be dried for sensitive reactions.

If you get fresh POCl3 from a chemical supplier you don't have to redistill it. But if you are using an old and opened bottle I would definitely do it.

terbium

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Re: trouble getting yields for LSD
« Reply #7 on: February 26, 2002, 04:25:00 AM »
Exactly which procedure are you following? Are you following the procedure in TIHKAL?


montanha

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Re: trouble getting yields for LSD
« Reply #8 on: February 26, 2002, 03:33:00 PM »
Thank you for your reply. My estimated yield for LSD from
LSA was about 1g from 3.15g. I'm sure it could be better. Maybe with fresh POCl3. I'm using an very old bottle without any purification.

The room (20m^2) is completely dark with one photographic redlight. There are blackout curtains at the window and the door has a light trap made from some blackout too.

I encourage you to do your own acid as it is very satisfying. In my life I decided to trip only by my own products so I had to do it.

montanha

  • Guest
Re: trouble getting yields for LSD
« Reply #9 on: February 26, 2002, 03:42:00 PM »
I'm trying the Shulgin method at the scale published in Tihkal. The only thing I changed on the original recipe was purifying the LSA by shaking with ether (not with the alcohol + ammonia).

I used CHCl3 HPLC which was anhydrous (<0.01% H2O). Oh, and it has some ethanol mixed to make it stable (~1%) but I think it's ok. I'm not sure about the water in MeOH (ouch) so I'll check it soon. Maybe this is why it's not crystalyzing.

I'll try soon cooking with fresh POCl3. Stay tuned.

terbium

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Re: trouble getting yields for LSD
« Reply #10 on: February 26, 2002, 05:40:00 PM »
For someone following the TIHKAL procedure, I would think that the 1% alcohol in the chloroform would be significant. (Assuming that this 1% is v/v) 150 ml of chloroform contains over a gram of alcohol, this could react with a significant amount of POCL3.

Is column chromatography of the LSD freebase being done?

Why is the LSD salt being prepared with maleic acid instead of tartaric?

Sunlight

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Re: trouble getting yields for LSD
« Reply #11 on: February 27, 2002, 01:31:00 AM »

terbium

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Re: trouble getting yields for LSD
« Reply #12 on: February 27, 2002, 07:49:00 AM »
Doing some calculations it would seem that the 1% ethanol in the chloroform is very significant. Using the TIHKAL quantities of:

150 ml chloroform
3.15 g lysergic acid hydrate (11 mmol)
3.4 g POCl3 (22 mmol)

The 150 ml of chloroform gives 1.2 gram (26 mmol) of ethanol. This is equivalent to the molar quantities of the reactants. I would guess that removing the alcohol from the chloroform would likely be much more beneficial to improving the yield than would distilling the POCl3.

slappy

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Re: trouble getting yields for LSD
« Reply #13 on: February 27, 2002, 03:42:00 PM »
Don't ever believe label claims about water content. Solvents always come wet. Especially the HPLC grade. For all water sensitive chemistry, they really need to be refluxed for ~16 hours over an appropriate drying agent like Sodium, Potassium, Sodium/Potassium Alloy (aka NaK), or Sodium/Benzophenone Ketal. THF comes so wet that you have to first distill it over LiAlH4, and then reflux!

For CHCl3, I would say to dry it with some freshly activated (still hot) 4A Molecular Sieves.

amalgum

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Re: trouble getting yields for LSD
« Reply #14 on: February 28, 2002, 10:27:00 AM »
My question is where did you get the precursor?  You don't have to answer that, but I wish I had your hook-ups:).

montanha

  • Guest
Re: trouble getting yields for LSD
« Reply #15 on: February 28, 2002, 04:57:00 PM »
Terbium, thanks for the lead.
We have cleaned our CHCL3 last night (wednesday) and now we are distilling it into an ambar bottle, we will finish drying brand new LSA and in about 3 hours we will start the addition.our POCL3 is already distilled from 2 days ago, and as soon as we get beautiful needles, I will get back w/ the good news.
I am thinking if its worth it to dry the methanol first... we are very excited, and we would like to thank everyone present in the board for the attention, repplies and sincere will to help us out and hear from our success.

Really, your efforts amaze me, guys.

THANKS A LOT  ;D

(and I am REALLY sorry for those looking for ET, but I'm not supposed to mention things about sources, and mine has made this clear to me - it's a matter of loyalty)  :(

El_Zorro

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Re: trouble getting yields for LSD
« Reply #16 on: February 28, 2002, 07:42:00 PM »
If it's not too much trouble, the Hive's been waiting for a pic of recrystallized LSD for a LONG time.  It would definately make a welcomed addition to every bee's photo library.

Lets see....Christopher Columbus, Charles Lindburgh, Neil Armstrong, and montanha.  One for the books.  Congrats.

I sell crack for the CIA

Vibrating_Lights

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Re: trouble getting yields for LSD
« Reply #17 on: March 01, 2002, 08:00:00 PM »
See if you can get a pic of the white light when you shake the crystals ;)
VL_

montanha

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Re: trouble getting yields for LSD
« Reply #18 on: March 01, 2002, 08:06:00 PM »
Well, I have made the addition, I have dried overnight and dissolved everything. Adding the maleic acid, I got a nebulous suspension, but I don't see needles yet. Not something filterable or weightable, just the same cloudiness I got the last time...Now it's happened quicker and it's definitely a lot more crowded. I hope this crystallyzation is slow, 'cause I cannot wait to see them beautiful crystals.

I guess that if it does not crystallyze absolutely by tomorrow moring, I will add a little ether. If it does not chrystallyze at all, I will guess that the methanol is not dry and will try to determine the yields in solution.

anyone w/ any other thoughts?

flipper

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Re: trouble getting yields for LSD
« Reply #19 on: March 01, 2002, 09:02:00 PM »
[off-topic]
If you just dissolve the acid freebase in some solvent Can't you just drop it on a sugar cube or is this only possible with a solution of the salt? Can you dissolve the freebase in water?[/off-topic]

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