Ergot Season is comming: Lysergic Acid from Ergot

[Dr_Heckyll]

This is an outline rather then a recipe; those who want to do it should have the skills to figure out the details themselfs; personally, I never conducted the procedure described, and never will. Lysergic acid derivatives are not my research interest.

All following steps after the grinding should be conducted with reduced light and/or in red light to avoid the formation of lumilysergic acid.

1. Collect a large amount of mature ergot (Claviceps purpurea) from infested rye fields. It is mature when it is quite hard and breaks almost like wood. (I wonder what happens to the ergot when rye is harvested/milled. Somehow it must be removed in order not to contaminate the flour. Is a flour mill a good place to get it in quantity?)

2. Grind the ergot to a fine powder, which will likely be a bit sticky due to the fat content.

3. Defat the ground ergot: thoroughly mix with some moist ammonium sulfate (10% by weight?) to fixate the alkaloids, then extract fats with nonpolar solvent: canonically hexane, maybe dichloromethane?

4. The alkaloids in the defatted ground ergot can now be hydrolized to lysergic acid and "goo", using KOH in water: stirr the defatted ground ergot for several hours, at elevated temperature, in a strongly alkaline KOH solution. Filtrate the alkaline solution. The filter cake can be disposed.

5. Now comes the magic trick. Follow

Patent GB1107156

: adjust the solution to pH of 5 - 7.5, add charcoal to the solution and stirr for one hour. Filter the charcoal off and elute the lysergic acid from the charcoal with methanol/ammonia.

6. Evaporate the eluate at 30°C/20mmHg. Suspend the dry residue in a small amount of water, filtrate and dry the so obtained crystalline lysergic acid in vacuum.

...and have a good excuse what you want with the ergot when you procure it.

Dr. Heckyll & Mr. Jive by Men at Work
...tells my tale.

[Ghost_Of_BT]

Have you dreamed this befor?

[sYnThOmAtIc]

Dude do you ahve any idea how much fucking sclerotum it would take to get a decent final product??? Do you know how much solvent your taking about to have to defat and extract alkaloids for this enourmous amount of shit?? YOu don't just take a walmart bag and go fill it up and buy a gallon of dcm and metahnol. Take a few contractor clean up bags and with todays fungacides and genetically altered seeds you'd have to cover a fifty square mile area to find enough to fill a small bag. There are much better ways of getting what your looking for... Not to mention the heat when you come back to your car and the officer siting there waiting asks, " Son what you need with two 55gal bags of contaminated rye that you just trespassed on private land to steal?"!

I belived he first said that he hasn't done this! And besides a good excuse if your lucky enough to find enogh ergot and unlucky enough to have to use it is that you resell it to researchers.

[bujinkan]

also take a look at the ergot identification guide, new on rhodiums site.

[hest]

All the stuff is at the tryptamine room. In one of the old article of acramon et al(50'/60') (don't have the ref right here, but im' sure I posted it before) They take some claviseps outside ther window, infect 100 sampel, to the most pink one, then infected 100 sampels and again took the most pink one. This strain now produced close to 2,5g LSA/L media (isolated yeald) I think that is the way.

[sYnThOmAtIc]

If you obatin a pure strain then you should not wast time infecting fields of rye or growing ergot! You can get 20g of lsa per 7-10days and 40-50g if you wait an additional 10days on that by submerged culture of the strain. Yields are based on minimum alkaloid production in 20 x 1L erlynmeyer flasks. Yields range from 1.2-2.8g/Liter depending on temp, o2 supply, nutrient mix, and days of culturing. In the patents it states that consistant yields are reproduced at 2.2g per 18days incubation at 25c. The culture medium is not that fucked up formula from psychadelic chemistry. It is very simple and consists of four or five ingredients which are very easy to get in large quantities for pretty fair price. Since alkaloid concentration is very high little solvent is needed to extract and is easily recovered and crystaline lsa stored. By starting multiple phases each delayed a period of time from each other depending on wheter you want to work up every week or two weeks. You can set it ip to where you harvest 20g a week or 50g every two weeks. Two weeks is better wastes less culture medium and is less workup plus oyu get much more the longer you wait. Idealy if you wanted to produce kg and move it fast you'd set up very large tanks and harvest every week.

-- The strains I'm refering to are radiation mutated strains.

[Dr_Heckyll]

sYnThOmAtIc: Take a few contractor clean up bags and with todays fungacides and genetically altered seeds you'd have to cover a fifty square mile area to find enough to fill a small bag.

This afternoon I went out, 10 minutes drive, and within 15 minutes I picked a nice bouquet of rye with beautiful sclerotia on it. I'll look for a way to make the pictures available. What I picked was chosen to look good, the cream of the crop. If I'd pick everything that's there, I could get about a teacup full in half an hour, maybe less. And that's not only one field, that grows all over the place. Maybe it's because ergot was and possibly still is cultivated in the area for the production of the peptide alkaloids? In this free European country there is no such thing like trespassing on agricultural property, and the farmer was plowing the field right next to it. He couldn't care less what I was doing.

The content of lysergic acid is low, yes, but there is quite a bit of ergotamine and ergotoxine in it, and that's why there is the hydrolyzation step, to convert these to lysergic acid. The nice thing about the method outlined is that it uses little solvent: the nonpolar for the defatting is essentially all. It is a small amount of charcoal from which the lysergic acid can be eluted with a small volume of methanol. And you know, smart people recycle their solvents insted of flushing them down the toilett.

MaDMAx: For aquisition of LSD precursor material, it would probably be easier to work on diversion of the material, or getting a hold of a modified strain and growing your own ergot with it.

Of course it's very easy to divert the material, and even easier to get hold of a modified strain. You just call 1-800-ATCC, right?

I estimate that 2 people in one afternoon can collect 2 kg. At an estimated total lysergic acid (i.e. including ergotamine and ergotoxine and other lysergic acid amides) content of 0.05% that's 1 g of lysergic acid. I don't need more than 2 liter of hexane or toluene to defat that in a Soxhlet. Pessimistically calculated, I recover 250 mg of lysergic acid. Shulgin achieved a yield of 66% LSD from lysergic acid, which would give me 165 mg. This is about 1650 doses. In my opinion that's not bad for an afternoon picking ergot   . A lifetime supply of LSD for one afternoon in the rye fields and a few more in the lab! Now beat this, dude!


Dr. Heckyll & Mr. Jive by Men at Work
...tells my tale.

[Dr_Heckyll]

MaDMAx: Well then by all means go for it!

I never said I want to go for it, and I actually said very clearly that lysergic acid amides are not within my research interest. I only wanted to post some information which seemed useful, particularly the charcoal-based isolation of lysergic acid from a large volume of solution. This technique can also be applied to solutions obtained from in vitro cultures, for example, or from the Convulvaceae. With your sloppy way of reading posts and lack of ability to see what really matters, I wonder how you got your title.

MaDMAx: Someone I don't know repeated the experiment with some random samples of ergot sclerotia to see if alkaloid extraction would be a feasible means of acquiring LSD precursor material.

Your better really don't know that bastard, because the analysis you are presenting here is bogus. Not the journal article, but those homemade or DEA-made or moron-made plots. You see, sometimes you meet your master, and I happen to have worked in the analytical department of a pharmaceutical company, received particularly training in chromatographic techniques. Someone absolutely wants to convince someone that ergot isn't a feasible source of lysergic acid, and I can only wonder why   . Where do you think Hofmann got his material from when he started to work on ergot-amines? Why did people develop ergotism from eating bread containing ergot, especially considering that the process of beaking will destroy most of the ergot alkaloids?

Patent DE0357272

from 1919 in example 2 starts with 2 kg of ergot and obtains the main alkaloid in an unspecified amount, but they certainly wouldn't have chosen to start with 2 kg if the yield was only a few mg. It's probably ergotamine what they obtained, which usually is found in a lower quantity then the other lysergic acid alkaloids together. Selected strains in 1919 when they didn't even know what to select for? Gimme a break!

And I can even beat you with your own weapon, the J. Chromatogr. paper: they found 3 alkaloids in every sample: ergonovine, ergocristine and ergotamine. Also, all samples contained more then one alkaloid. Yet, someone you don't know found none whatsoever? And you believe that?  

Just from looking at the numbers, the MS strain seems to have about the lowest content: 12.4 µg/ml total alkaloids, not counting the wrong-isomer -inine compounds. This is 0.0124 %. Not great, but the material is for free, safe to acquire and easy and cheap to extract.

It was hell to figure the actual percentage out, because there is something freaky wrong: what should be mg reads on my monitor as µg, yet when I copy and paste it here, it's correct:

2.2. Extraction and sample preparation
One hundred mg of crushed ergot of rye were extracted with...

What the hell is going on here? When you look at the article on your computer, do you see mg or µg? I have a screen shot to proove the µg on mine...  

An average strain, FS, contains 130.95 µg/ml, or 0.131 % total lysergic acid alkaloids. That's not bad! It also fits well to my original informed guess of 0.05 % lysergic acid and verifies my calculations. And with these facts some morons are trying to tell us that it's not worthwhile to use ergot as source of lysergic acid? It might be in the DEA's interest that we believe that, because it's just so much easier to get caught when trying to divert ergot alkaloids or acquire a selected strain...

Sorry, but I have to give you a big thumbs down: If you want to be an A+ Analyst you should get a critical mind of your own and get your facts straight...or move your rotten ass out of here, DEA agent MaDMAx. The Hive, knowing you far longer and far better than I, will be able to determine what you are: a moron or an undercover, or still an A+ Analyst for qualities I haven't seen on you yet.

Some will probably criticize me for going so harsh against you, MaDMAx, but it's exactly people like you with their pseudo-knowledge and/or disinformation who are hampering our progress. Without really knowing, you just dismissed ergot as source of lysergic acid, and did whatever you could to keep me from trying it, discouraged everyone with smart psychological tricks: Do some sort of analysis first to make sure you don't waste your time, you recommend. Which bee has even a remote chance to get an analysis done? Of course, you wouldn't mention that such an analysis could be done with low tech: TLC for example. Or simply extract some ergot on a test-tube scale. Then a few tests to verify and roughly quantify (by comparing with known strength solutions prepared from an ergotamine tablet) the alkaloid content can be applied: the peptidic alkaloids show light blue fluorescense under UV light (365 nm, easily available). Maybe that could even be used on the ergot itself? The Keller and van Urk colour reactions are two chemical tests. But instead of drawing the attention towards those easily availabe tests, you make it look like the only way to do it is via some high-tech mumbo-jumbo chromatographic stuff to which 99.999% of people interested in making LSD have no access to. All availabe information indicates that 2 kg of ergot will produce at the very least about 100 mg of lysergic acid, yet you are implying that it would likely be a waste of time. Why are you pressing so hard to discourage when all facts are very encouraging?

If I wouldn't have proven you wrong in every point you made, enabled through my professional training, The Hive would have followed your argumentation and dismissed ergot as a source of lysergic acid once again, and the illusive dream of a selected strain or diverted material would have continued. And those interested in making LSD would have once again missed the most easily and safely available source of lysergic acid, the source the father of LSD used!


Dr. Heckyll & Mr. Jive by Men at Work
...tells my tale.

[bujinkan]

dr heckyll lay off the steroids, madmax's post serves as a good reminder of the need for strain isolation and analysis...of course ergot is a great source for precursor, and i seriously doubt that madmax's intention was to say that it wasnt.  its a well known fact that alkaloid content varies from strain to strain, and if i wasnt so tired id go look for something that brought up even more variables for alkaloid content...like perhaps the maturity of the sclerotia, maybe even the host organism.
In any case, you shouldnt get on swimax for experimenting or hypothesizing. lsd synthesis needs to be discussed and all angles need to be examined.

[Dr_Heckyll]

bujinkan, you edited your post while I was writing a reply. I can't waste my time on games like that, especially as you didn't even make clear what you edited...

Here is your original post:

dr heckyll lay off the steroids, madmax's post serves as a good reminder of the need for strain isolation and analysis...of course ergot is a great source for precursor, and i seriously doubt that madmax's intention was to say that.

To that one I can agree: it is not madmax' intention to say that ergot is a great precursor (source of lysergic acid).

Does madmax need you to do the backpaddling for him? Or are you madmax' alter ego as you seem to know so exactly what his intentions were? Isn't he man enough to say: Heckyll, you *%&$, you are talking one pack of shit and I can prove it: here you say this but it is so because of that? Once you prove me wrong I'm the first to admit it, and I've proven that. But you just step in and light a couple smoke candles to blur the vision for the facts.

In your edited post, you already start casting doubt in many bees minds again: the maturity here and the strain there and whatnot elsewhere. Why do you try to spread confusion again? Why don't you stick to the basic facts: if someone is in need of lysergic acid, he best goes, in late July to early August, collects 2 kg of ergot, so it is abundant in his area, and extracts it according to a certain, very easy and efficient methods and this way obtains at least 100 mg of lysergic acid which he can convert to a lifetime supply of LSD? Stick to the facts, stick to the basics AND FOR ONCE LET BEES GET THINGS DONE INSTEAD OF JUST PALAVERING....and spreading insecurity I should add.

Dr. Heckyll & Mr. Jive by Men at Work
...tells my tale.

[hest]

Dr_Heckyll MaDMAx doo know wath he is talking abouth.
Don offend bees before you have read atleast some of their post's

[bujinkan]

bujinkan, you edited your post while I was writing a reply. I can't waste my time on games like that,

i doubt that anyone will take the time compare the two posts, and theyll likely take your word for it, but i was fixing a typo and adding a few more lines. My standpoint on the issue was clear however...look at the first few lines.

Does madmax need you to do the backpaddling for him? Or are you madmax' alter ego as you seem to know so exactly what his intentions were? Isn't he man enough to say: Heckyll, you *%&$, you are talking one pack of shit and I can prove it: here you say this but it is so because of that? Once you prove me wrong I'm the first to admit it, and I've proven that. But you just step in and light a couple smoke candles to blur the vision for the facts

you, my friend, have been smoking too much crack. This is the second time your rediculously unwarranted aggression has blinded you to the actual point of someones post. You are trying to make a war where there is none..no one is trying to crush your dreams, I am just acknowledging madmax's point that strain analysis should be done before you invest a large amount into untested claviceps strain.

In your edited post, you already start casting doubt in many bees minds again: the maturity here and the strain there and whatnot elsewhere. Why do you try to spread confusion again? Why don't you stick to the basic facts: if someone is in need of lysergic acid, he best goes, in late July to early August, collects 2 kg of ergot, so it is abundant in his area, and extracts it according to a certain, very easy and efficient methods and this way obtains at least 100 mg of lysergic acid which he can convert to a lifetime supply of LSD? Stick to the facts, stick to the basics AND FOR ONCE LET BEES GET THINGS DONE INSTEAD OF JUST PALAVERING....and spreading insecurity I should add.

have you lost your mind? are you seriously trying to pawn off the idea that alkaloid content never varies according to strain?
and whats your reasoning behind ignoring what should be common sense: because it makes people unconfidant in using ergot as a precursor. this is rediculous. come back and reread the posts when you arent drunk.
And then you say that i am spreading smoke and talking nonsense...the sad thing is that my posts rarely get read at all, even though the contents are usually well thought out and valid, so everyone will probably believe you. But for your sake ill reiterate the points once again..
-alkaloid content varies from strain to strain in claviceps purpurea.
-it may also vary due to other factors.
-this doesnt mean it cant be used, those are just fact that any bee should be aware of

I suggest you look at the thread ergot and agar. do a search.

[obia]

I figure that going to a grain store with a gravity separator at the right time of year you could get 100's of kilos of ergot. surely the clay absorption method reduces the qty of organic required to trivial levels, the only problem is then how to homogenise the ergot prior to extraction with aqueous acid.

[locrian]

the sad thing is that my posts rarely get read at all, even though the contents are usually well thought out and valid, so everyone will probably believe you.

Not true, B.  I read your posts and have respect for your thoughts.  Without looking at the Hive, I can probably write down a good handful of screennames just from memory, just from having seen the names so many times.  You would be on the list, Heckyll would not (no offense, just making an observation). 

On this board, having credibilty is very important.  (I mean who you gonna believe, "Rhodium", or "CraZayGluSnifr"?)
Besides the moderators, there are quite a few bees that shine - whose advice I would trust for the most part.  There have been times I posted something and get a response from someone and then go back and search for the username sorting oldest first and read through posts that person has made.  Just to see if they know what they're talking about and "feel out" the person through their posts.  Known dumbasses and people whose posts I never happened to read I'm skeptical about.  Most known dumbasses sign up for a new name after their stupidity or bullshit lies become apparent, so strangers and newbees I'm skeptical about also.  This is just the respect system on the Hive and I think we all know that. 

Anyways, yes back on topic a little here - isn't this process of ergot acquisition dangerous, b/c I think I remember reading that one runs the risk of getting gangrene or something like that while cultivating ergot.  Perhaps that's just from the process of cultivating your own or someone might have mentioned it by now.

[terbium]

Anyways, yes back on topic a little here - isn't this process of ergot acquisition dangerous, b/c I think I remember reading that one runs the risk of getting gangrene or something like that while cultivating ergot.  Perhaps that's just from the process of cultivating your own or someone might have mentioned it by now.
Nah, I think that is just a myth. I believe I have read (Perhaps in Hofmann's book) that before submerged cultivation was developed collecting ergot from the fields was done by children.

[bujinkan]

terbium, locrian...are you two serious? remember st anthony's fire?  dont handle claviceps purpurea without gloves.
locrian, thanks, nice to know that im read.

[hest]

I'v been working with ergot culture without glowes(liquid and agar) and havent's  seen Skt. Anton yet.
Acramonn don't say anyething abouth it either.

[locrian]

Just re-read this thread sober.  Very interesting, although you were overboard just a bit there, Heckyll.  The DEA shit was funny, though.  Well if he is a DEA agent, he's the best damn agent they have (or maybe the worse?).  Fooled all of us - and taught swinl more than a thing or two about orgo. lab! (And I don't think I'm the only one who appreciates all his contributions to this site and field of study.)  Thanks for the help, DEA, we owe you one!  And he picked a damn good name - I mean, you know, for an undercover agent posing as a bee.     Very clever black n' decker.

Dr. H., You seem pretty convinced that most if not all wild growing (if you will) ergot will contain a decent enough amount of alkaloids to make a random trip to the nearest rye fields worthwhile.  MaDMAx disagrees quoting that studies seem to indicate most ergot is worthless for alkaloid extraction.  So where does the truth lie?  MAx, got any info on where good ergot grows then, how to obtain, or maximize content?  What causes the alkaloid content to be high or low - the rye, the length of time it has grown, what?  You know, kinda like how Brazilian Sassy is supposedly prefered (having less "pre-run"), or how some MHRB doesn't have hardly any DMT, or like how some regions have wild growing weak to moderate mushies, but others have the dank ones, etc.

Heckyll - do have any kernal of knowledge that would convince someone enough to just go try this? - convince me it would be worth a bee's effort.  ie - how are you sure that most ergot is worth extracting alkaloids from?  (Damn, excuse the preposition ...)  Just from what you've posted, you sound somewhat convinced yourself, but its not your field of interest you say.  Really?  You sure seem passionate about it.  But I guess not since you say you're not - the same as all of us seem to know this cat, SWIM, he's a cool guy.  I'm just playin' though, I believe you, or you probably actually wouldn't give a damn about this sort-of-debate.  I mean, wasting time, energy and money REALLY sucks (take it from swinl - had bunk Sassy recently, fucking pigs!), plus debatingly risking gangrene (ok probably not, but still) for a worthless experiment also would suck.  MaDMAx really was just trying to prevent crappy shit like this from happening (thanks, 'MAx!).  Don't leave the thread on a sour note, brush the chip off and share your knowledge, I was listening ...

[Rhodium]

This is also interesting reading:

https://www.thevespiary.org/rhodium/Rhodium/pdf/ergot.alkaloids.chem.rev.pdf

[Dr_Heckyll]

Locrian, lysergic acid derivatives are not my research interest, because I'm exclusively looking at legal to manufacture compounds. For me that's kind of part of the game. I'm working on a different basis than most bees and with a different objective, so legality does matter for me. I'm passionate, yes, because someone is trying to cover the truth under some crappy analysis. (Where is the baseline drift comming from, not seen with the positive sample? Why is there no noise in the signal, no spurious signals from various basic compounds necessarily found in ergot? What weird shape of peak is this, invented super-chromatography? Why does even the paper look different? How can you expect to get a good signal above noise with twice the amount you get none at all; at least x 10 would be necessary? The decomposed sample, btw, looks more "real".)

Yes, I'm convinced that every ergot sample is a viable source for lysergic acid (LSA), although maybe not for large-scale production. One would have to be extremely unfortunate to find no useful LSA content. I did read over the paper Rhodium just posted, but I didn't see and relevant information; I have to re-read it more thoroughly though.

Heckyll - do have any kernal of knowledge that would convince someone enough to just go try this?

I thought I made my case. Even the paper Madmax cites indicates a usable content in their worst sample. I suggested some simple means for preliminary tests. Sorry I can't give you a reference guaranteeing that every ergot sample will contain at least x % of LSA alkaloids.

Are you all aware that it's the LSA alkaloids which cause the gangrene / St. Anthony's fire (I called it ergotism)? You are worried about gangrena from ergot, and at the same time that it contains no LSA alkaloids? Spock would call this extremely illogical.

All right, I was overboard re madmax, but I couldn't understand how someone could possibly be so predjudist, elitist and blinker minded, trying to proof with some crappy analysis that ergot collected in a random rye field is not a valid source of LSA, not even properly analysing the literature he cites...and everything but dismissing ergot completely based on one failed analysis.

Btw, I never claimed madmax IS a DEA, and if I did so please tell me where. Madmax, you're rediculous with your new signature. Again, you're showing your lack of analytical skills   .

A big battle would be won in the war against the war if ergot could be proven to be a vaild source of LSA.

I could help to do that in two ways:

1. Supply to one serious bee in Europe 2 kg of Secale cornutum collected in my area. (Looking forward to a small sample of the finished product in return   .) Shipping ergot to the US is just no feasible.

2. Help to establish a simple procedure to estimate the LSA alkaloid content of ergot, using the methods I mentioned earlier. EDIT: I just noticed that bujinkan in

Post 338166

(bujinkan: "Heres the above post by mountain girl in readable", Tryptamine Chemistry) seems to have started looking at that option already. Hint: hydrolize alkaloid mix to LSA, use TLC, develop with van Urk. Can be used on crude extract in test tube, but tryptophan will interfere.


MaDMAx is not a DEA but an A+ Analyst wearing blinkers instead of sunglasses to look cool