Author Topic: LSD synthesis  (Read 5999 times)

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crysalis

  • Guest
LSD synthesis
« on: October 20, 2004, 03:59:00 AM »
I realise many forums look down upon people staring threads for their first post although i've been searching for the last two days  for a reliable, not overly complex synthesis of LSD and am having a nightmare.

I originally found great promise in this synth on Rhodiums site:

Preparation of Lysergic Acid with Sodium Hydroxide Alone

5g of paspalic acid in 100 ml of a 2N aqueous solution of sodium hydroxide are heated at reflux for 2 hours. After cooling, the pH of the reaction medium is brought to 5.5 by adding an aqueous solution of hydrochloric acid and glacial acetic acid (20 ml of water, 10 ml of HCl and 10 ml of acetic acid). The precipitate is filtered, washed with 3x20 ml of 50% aqueous methanol, then dried in vacuo at 75°C. This gives 3.15 g of lysergic acid comprising 6.8% of isolysergic acid and the yield (w/w) is 59.3%.

This seemed all to easy until I researched a lot more and found paspalic acid is impossible to obtain unless I want to venture into fungus cultivation.
I've also been slightly detered by everyones comments that LSD is one of the hardest drugs to synth and no one on this site has succesfully attempted it.

Please, I am very motivated and have learnt quickly over the last few days of my research yet require those with experience to giude me further as i've hit a wall due to my relative newness to this field, can anyone suggest a reasonable synth? I can easily aquire reflux and vacuum stills, magnetic stirrers, most chems, etc and have a few people willing to finance this venture and I will be happy with a rather poor yield.
I hope you don't see this as spoon feeding because I have searched and read for hours.

java

  • Guest
Ref: Synthesis of LSD......
« Reply #1 on: October 20, 2004, 07:11:00 AM »
Here is a nice list of references with the articles that may be of help to you....java

Post 525552

(Lego: "First direct synth of (+)-lysergic acid, Refs", Tryptamine Chemistry)



crysalis

  • Guest
alkaloid precursers
« Reply #2 on: October 21, 2004, 05:51:00 AM »
So regardless of my method I am going to be required to brush up a bit on my aseptic culture techniques? The only synths i've seen have used ergot alkaloids grown in culture to extract LSA, this then involves bonding it with diethylamine also.

I remember scanning over a source that said hawaiian baby woodrose seeds offered a good precurser to LSD so I searched and found Michael Valentine Smith's Psychedelic Chemistry which gave an interesting write up on extracting lysergic acid from HBWR. Yet what caught my eye was Hoffmans LSD via Hydrazide, it's a direct synth from ergotamine to LSD without having to extract lysergic acid yet again I cant find a source of ergotamine and its included on the banned substances list for Australia so I cant order it overseas. It would appear woodrose is the best option although prices for the nervosa variety are $1,400 a kg, enough for a gram of LSD which is unfortunatly just slightly out of my price range.

Any suggestions of a economical precurser? Advice on a cheaper source of woodrose would also be greatly appreciated.

And thanks for that link java it most definetly helped.

indole_amine

  • Guest
hbwr
« Reply #3 on: October 21, 2004, 07:30:00 AM »
For cheap HBWR wholesale retailers, search the internet.
They can be had for 400 bucks/kilo...

(besides, 1400$ for 1 gram of LSD is damn cheap! As it will last you for the rest of your life!  ;) )

Then read

Post 527262

(n00dle: "LSD vs peptide coupling", Tryptamine Chemistry)
and UTFSE for "argyreia nervosa" and/or "HBWR", maybe together with "alkaloid extraction".

Good luck.


indole_amine

Drug_Phreak

  • Guest
Do you have any refs for growing Ergot ...
« Reply #4 on: October 21, 2004, 06:00:00 PM »

java

  • Guest
Heavenly Blue...morning glory gate to LSD
« Reply #5 on: October 21, 2004, 06:34:00 PM »
Why don't you grow some morning glory flowers and harvest the seeds, there is a variety that has a high ergot amount , I think they are the heavenly blue . Make it a trallis and grow it on both sides it's a hardy plant and it will give you enough ergot material for your project...........java


Drug_Phreak

  • Guest
Most of what I found in TFSE regarding this...
« Reply #6 on: October 21, 2004, 08:18:00 PM »
Most of what I found in TFSE regarding this seems to be nonsense. You can't just add a few Ergot strains to a culture medium and expect it to produce a large amount of LSA like you find in Ergot fungus that has been grown on rye etc. Especially in some makeshift laboratory filled with contaminants. Valentine’s culture seems rather crude also. From 2.2 pounds of HBWR you should expect about 0.4 - 3 grams of LSA. Try to get seeds that where actually grown well in Hawaii. Yeah, Morning Glories are a cheaper way to go, but you'll need roughly 2 - 3 times as much seeds. The ones that are highest in LSA are Heavenly Blues, Pearly Gates, and Flying Saucers.


Rhodium

  • Guest
restrict critical searches
« Reply #7 on: October 21, 2004, 08:57:00 PM »
Most of what I found in TFSE regarding this seems to be nonsense.

Therefore it is a good idea to restrict critical searches like this one to only include posts which has been up-rated (see the checkboxes in TFSE).


crysalis

  • Guest
Re: UTFSE for "argyreia nervosa"...
« Reply #8 on: October 22, 2004, 02:51:00 AM »

UTFSE for "argyreia nervosa" and/or "HBWR", maybe together with "alkaloid extraction".




I have searched thats why I stated it as a viable source of LSA. Also theres an extraction method in Smiths book for ergot and woodrose.

Additionally woodrose has been found to have the highest concentration of LSA, heavenly blue and morning glory have 0.02% LSA while woodrose has 0.04%. It is also determined by which variety of nervosa you use, HBWR has been found to have the highest concentrations as stated on this site

http://www.shaman-australis.com.au/Website/subcat25.htm

(it seems reliable enough).

Where have you managed to find a kilo for $400? Also which currency is that? I've thought extensively about ergot culture although I don't have a clue where to track down a rye farm or another source of ergot alkaloids. And after that actually growing a enough of a culture to provide enough of the precurser is a whole challenge in itself. No one in oz happen to have a few woodrose plants growing out back would you? Because that seems like my only reasonable option.


indole_amine

  • Guest
..Oz? Hot summer? - Grow'em!
« Reply #9 on: October 22, 2004, 03:18:00 AM »
I actually don't remember the site anymore; I probably didn't try to memorize it at all, because of the fact that I had found it with google searching for "HBWR" - that's for sure.

I think it was a company located in N.Y./USA, they had four different strains and qualities, I figured back then that the medium quality seeds should work fine, but then again, now I'm unsure if it was 400$ for half or 1 kilo...

Anyway, they can be bought for reasonable prices (even 400 bucks for 0.3g lysergic acid seems like a very reasonable price, even 500 are fine, if you count the reagents needed for extraction and hydrolysis/isomerization.

But since you live in oz, growing virtually thousands of HBWRs should'nt be a problem for you: or do you live in one of the five(?) big cities? Then you have bad luck with growing... Else you should have enough free space, and the weather should be fine, too - at least around summertime/christmas..

(funny country you have!  :) )

No, really: I suspect that you have a quite subtropic climate during summer, so the woodroses can probably even be harvested twice a year, and they for sure contain lots of LSA when growing under such optimal conditions. Growing is by far the cheapest and least suspicious way - if you don't live in a city, that is.


indole_amine

crysalis

  • Guest
Damnabit'- although theres hope
« Reply #10 on: October 22, 2004, 03:44:00 AM »
Unfortunatly I do live in a city :(  although I may be able to find a few areas to grow it in, especially an old drive in movie theater near me; good sunlight and large area although I may have to set up a trellice(sp?) seeing as though there are few things for it to climb.

Thanks for the suggestion indole_amine, that site I linked sells already sprouted plants which could shave some time off although now i need to learn how to extract the seeds and how to initiate seeding. Any idea how many would be in a plant? I highly doubt i'd be lucky enough to get a kilo from a plant although I can dream :P , perhaps three should do it.

This extraction method seems reasonable, again its from Smith:

Extraction of Lysergic Acid Amides from Woodrose Seeds or Powdered Ergot

Reduce the seed material to a fine powder in a blender, and spread it out to dry. Grind it again if it is not fine enough after the first time due to dampness. Saturate the powdered seed material with lighter fluid, naphtha or ligroine. When completely saturated, it should have the consistency of soup. Pour it in a chromatography column and let it sit overnight. Remove the fatty oils from the material by dripping the lighter fluid or other solvent through the column slowly and keep testing the liquid that comes through for fats by evaporating a drop on clean glass until it leaves no greasy film. It will take several ounces of solvent for each ounce of seeds. Mix 9 volumes of chloroform with 1 volume of concentrated ammonium hydroxide and shake it in a separatory funnel. When it settles the chloroform layer will be on the bottom. Drain off the chloroform layer. Discard the top layer. Drip the chloroform wash through the column and save the extract. Test continuously by evaporating a drop on clean glass until it ceases to fluoresce under a black light. Evaporate the chloroform extracts and dissolve the residue in the minimum amount of a 3% tartaric acid solution. If all the residue doesn't dissolve, place it into suspension by shaking vigorously. Transfer the solution to a separatory funnel and wash the other vessel with acid in order to get all the alkaloid out. Pour the washings in the funnel also. Basify by adding sodium bicarbonate solution, and add an equal volume of chloroform. Shake this thoroughly, let it settle, remove the bottom layer and set it aside. Once again, add an equal portion of chloroform, shake, let it settle and remove the bottom layer. Combine the chloroform extracts (bottom layers) and evaporate to get the amides.

bbell

  • Guest
morning glory no ergot
« Reply #11 on: October 23, 2004, 04:09:00 PM »

java

  • Guest
Discussion on Synthesis of LSD
« Reply #12 on: October 23, 2004, 05:51:00 PM »
Here is more information found at the Rhodium  Chemistry Archives


....LSD commonly is produced from lysergic acid, which is  made from ergotamine tartrate, a substance derived from  an ergot fungus on rye, or from lysergic acid amide, a  chemical found in morning glory seeds





............as read at

../rhodium/chemistry
/lsd.synthesis.html






violethorn

  • Guest
My opinion
« Reply #13 on: October 24, 2004, 09:50:00 AM »
Making the hydrazide seems to be the most convenient method. Originally Hofmann used hydrazine hydrate and then at some point switched to anhydrous hydrazine. I imagine the yield is slightly better. However, pure hydrazine is used as an ingredient in rocket and jet fuel. It's hard to aquire, twice the price of the hydrate, much more volitile, more toxic and has a much shorter shelf life.

As far as your starting ingredient for the lysergic acid, I've no experience with HBRW seeds, but it sounds like a slim margin. What you want is ergot. A little goes a long way. SWIM sells it for forty dollars a gram. Canadian. bulk deals send private message. The neat thing is that when you have ergot you have the fungus Claviceps purpurea. Simply break one ergot open and scrape out some of the off-white substance in the center. It reproduces well on potato dextros agar which can be purchased from a microbiological supply store, or made yourself.


indole_amine

  • Guest
bullshit
« Reply #14 on: October 24, 2004, 10:37:00 AM »
"Making the hydrazide seems to be the most convenient method."

Surely not! There are several other synthetic routes using less dangerous reagents AND offering better yields, this includes for example the carbonyl diimidazole (CDI) method, as well as the different peptide coupling reagents like DCC and pyBrOP...


"What you want is ergot."

You want everything else but ergot. You want lysergic acid, which is not ergot. Ergot just produces lysergic acid, but the amount is very small, too (unless you have the skills of isolating a high-yielding strain  :P ). It further is toxic, will cause gangrene, most surely it is NOT one of the high yielding strains, and it still has to be cultivated in liquid media, and then there is the solvent extraction of several liters of mycelium-loaded liquid... :(  - And risking the hazards of handling and storing big volumes of toxic and/or explosive solvents, together with the risk of a claviceps intoxication (in fact one of the things that normally require "biohazard" signs and closed lab doors!  :o ) is NOT what you want, believe me.

At least not if you plan on making some acid for you and your friends. There are scientists at Sandoz spending their whole lifetime with cultivating highly mutated special claviceps strains though, so this might be the way to go if you're more into spending your whole life with cultivating toxic fungus and harvesting it... ::)


indole_amine

violethorn

  • Guest
Bullshit Not!
« Reply #15 on: October 24, 2004, 03:02:00 PM »
I wasn't talking about synthesizing lysergic acid with hydrazine. In fact, I wasn't talking about synthesizing lysergic acid at all. That's a very long and expensive procedure (my opinion). What I was talking about was extracting lysergic acid from material that occurs in nature, namely ergot, with hydrazine.
Ergot contains lyergic acid not in its pure form but in one of it's derivatives (ergot alkaloids). Ergot alkaloids are lysergic acid bonded with an amino acid. Which amino acid it is bonded with determines which alkaloid it is.
Treating any ergot alkaloid (or a mix) with hydrazine (anhydrous or hydrate) will result in the bond between the lysergic acid and the amino acid to be broken, the amino acid to be garbaged, and the lysergic acid to be immediately bonded with the hydrazine into iso-lysergic acid-hydrazide, which crystalizes. Thats my understanding of what occurs. You don't obtain lysergic acid in it's pure freebase form, but you don't kneed to. Then, you go from iso-lysergic acid hydrazide to LSD.
The fungus Claviceps purpurea is the cause of ergot occuring in nature. The fungus secretes the alkaloids as a by-product of it's life process.


indole_amine

  • Guest
?
« Reply #16 on: October 24, 2004, 08:31:00 PM »
Hydrolysis can be done with any strong base, KOH is often used here. The hydrazine method is a bit outdated. And ergot is dangerous. Its the alkaloids that are the dangerous substance, and you're after the alkaloids, so you're doing a dangerous job. Get it??? (side note: LSA="lyserg saure" amine=lysergic acid amine, which is NOT that dangerous at all...)


indole_amine

n00dle

  • Guest
There are neumerous (spelling?
« Reply #17 on: October 25, 2004, 02:53:00 AM »
There are neumerous (spelling?) threads on why ergot is -not- any more dangerous than other chemical preps if done correctly.

Yes, the products from ergot cultivation (alkaloids) can cause gangrene, but, this must be ingested in huge quantities. This would be the same as a migraine sufferer downing like 10 packets of ergotamine tablets.
If you are stupid enough to eat a brunch of brewing bulbbling gross stuff, you probably deserve to get what comes to you.

In regards to ergot cultivation, unless the -spores- cause inherant danger when inhaled, then this might cause an issue. But nobody has posted anything on this.

An ergot setup with HEPA in, and bleach bubbler out, will suffice. as long as you dont eat your product.

Also, a question SWIM has wanted to ask for a while.
Yes, woodrose contains the highest concentrations of LSA compared to morning glories, but, we are interested in -any- hydrolysable ergot alkaloids. What if the ergot alkaloid profile of a morning glory was like, 99% ergot alkaloids (unpsychoactive) and 1% LSA?
This would make MG's more suitable for a starting material. SWIM will look up alkaloid profiles for both now, but would appreciate if anyone has this information, to post it.

Astrum

  • Guest
Yeah, from what I've read you have to work...
« Reply #18 on: October 25, 2004, 03:24:00 AM »
Yeah, from what swim has read you have to work with large amounts of ergot without proper protection over a period of time before it gives you gangrene or anything serious like that.

Still, working with LSA would be safer by default even if doing micro-batches. That peptide coupling thread a few threads down looks like an interesting process. Of course getting BOP or PyBOP wouldn't exactly be a cake walk. In either case I think LSA would be the better way to go as opposed to ergot. Of course you need to know your chemistry and chemistry techniques if you want to do it. I believe that the peptide coupling procedure requires chromatography, or atleast last time I checked it they were talking about that (haven't checked it in quite a while). I also know a few places to get cheap seeds, not going to name names but there are sources out there. And even if you do have to pay $1,000+ per Kg (not sure what currency you're using), the return will be quite high. Besides, trying to produce ergot would be a huge pain in the ass. Just my opinions though.


hest

  • Guest
Ergot
« Reply #19 on: October 25, 2004, 04:18:00 AM »
I have been working with Ergot in a otc setup (cottonplug's ect) and I'm not dead or become a warewolf (atleast not more than once a month')