Author Topic: LSD from HBWR  (Read 1352 times)

German

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LSD from HBWR
« on: December 03, 2009, 08:49:05 PM »
Anyone try extracting the %0.25 LSA and other LSD amides from HBWR seeds and then converting to LSD-25? I think this is going to be my next project and I just want to get feedback from anyone who may have attempted it before. The Erowid vault is the best source I've found so far but even their couple writeups seem to be questioned by some as the best way to go about it.

Naf1

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Re: LSD from HBWR
« Reply #1 on: December 03, 2009, 10:36:51 PM »
Could you post the write ups you are looking at?

German

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Re: LSD from HBWR
« Reply #2 on: December 03, 2009, 10:56:00 PM »
Part 1

First you do one of these two LSA extraction methods:

The method is very simple, requires nothing you can't buy easily and legally, and it's not very expensive. There are refinements galore to this, and I might try them in order to purify this stuff, but the chemicals aren't as available, and it requires things like pH paper, which I don't know how to get. Maybe I can get some anyway. I'll see.

First of all, you need either (a) a lot of morning glory seeds or (b) some hawiian baby woodrose seeds. You also need petroleum ether, which is a petroleum refining byproduct, and some high proof drinkable ethanol.

I'll explain the theory as I understand it so that you can understand the flexability in this recipe.

There are two kinds of solvents, polar and nonpolar. Generally, the good stuff in seeds is polar soluble, and the bad stuff is nonpolar soluble.

So the idea is to first make a nonpolar solution, which of course means that you take a nonpolar solvent and soak the ground up seeds in it. The result is a solution of garbage from the seeds and the nonpolar solvent. Petroleum ether is a nonpolar solvent, so it will function in this capacity. The down side is that petroleum ether is poisonous, so you don't want to drink it. The good news is that pet. ether is extremely volatile, so it evaporates quickly and cleanly. So the first stage is to soak the ground up seeds in petroleum ether for a few days, and then filter the resulting cloudy solution through some coffee filters, throw away the solution, and keep the seed mush. The seed mush consists of nondisolved LSA's, fiber, and the remaining solution that didn't drip through the filter. This part can be iterated to get more and more garbage out of the mush. The final time, let the seed mush dry thoroughly so that the petroleum ether evaporates and you don't have any poison in there.

After the seed mush dries, the nest stage is to make a polar solution, which separates the alkaloids (the LSA) from the fiber of the seeds. This is done with alcohol. There are other polar solvents, but again, the key is to have one which easily evaporates, one which will not destroy the LSA's, and one which is not poisonous. Ethanol serves this purpose. Methanol will also work, but methanol causes blindness, so if you use methanol, make damn sure it's all evaporated before consuming the product. In some states ethanol is illegal, and California is such a state. In that case, using methanol is probably the way to go. Also keep in mind that there is such thing as denatured ethanol, which is ethanol which has been intentionally poisoned so that it is undrinkable. The reason for doing this is that drinkable ethanol is taxable under the Tobacco Alcohol and Firearms people, and denatured ethanol has uses in chemistry and cleaning. The point is that you should under no circumstances use denatured ethanol because it will make you sick or kill you or cause cancer or all three. So, make an alcohol solution of the seeds. Then filter the solution through filter paper, like before, except this time keep the liquid in a jar. Repeat this step 3 or 4 times, always keeping the liquid. When you've exhausted the seeds, throw them away. The liquid you have should be yellow and smelly. Put this in a shallow flat tray or pan or large bowl, and let it evaporate in a dark dry place for a day or two, or until there is no liquid. The pan should have a yellowish scum residue. That's the LSA gunk. Scrape that up with a razor blade or credit card or whatever works. It'll be sticky and gummy, and once it's all scraped up it will look dark brown.

That's pretty much all there is to it. You can take this several steps further to get a more pure product. That would be to alternately make an acid solution and base salts from the LSA's, which would eventually leave you with a very pure white powder. This requires much more effort, and wastes some of the product, and the only reason for doing it would be to remove more garbage, but the amount of garbage left in the brown gunk is insignificant.

Once you have this stuff as pure as you want it, you can ingest it in your favorite form. You can either swallow it as a lump, put it into a gelatin capsule, drink the ethanol solution, or dissolve it in some cool-aid. I recommend either capsules or swallow the lump if you can handle the taste.

Other notes: Petroleum ether is in Naptha, which is available in hardware stores. That's what I've used, and it works fine. [However, see this warning about Naptha] Other petroleum solvents would work like ethyl ether, which evaporates much more easily and is a better solvent, and something like gasoline, which has additives and does not evaporate as cleanly as naptha. If you can get petroleum ether from a chemical supplier, try it instead of naptha. A rule of thumb is that after making a solution with the nonpolar solvent, and after it dries, it should smell absolutely nothing at all like petroleum, or whatever solvent you used. If you use gasoline, you'll notice a strong gasoline smell, which means you're screwed. I know first hand from repeated experience that naptha works. Also, read the labels of whatever solvent you use. Make sure it contains no benzene. Benzene is the most evil carcinogen known, and even in trace amounts it can cause cancer. There is no safe amount of benzene. On the other hand benzene is everywhere, and if some chemical engineer points out to you that there is benzene in naptha even if it's not on the label keep in mind that there is an enormous amount of benzene in automobile exhaust. You're going to die anyway. If there is no mention of carcinogens or benzene on the label of the naptha, then there isn't enough such that you should not use it.

The finer details of this recipe I can give you another time, but I just wanted to give you some theory and a general idea of what the procedure is. I can give you some things I have from off the net pertaining to this.

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Subject: Re: Extracting LSA from HBWR

Concerning the extraction and purification of LSA from HBWR, The alkaloids are
more polar than e.g. DMT or mescaline, and are probably water soluble to some
extent. Thus, while a crude extraction can be performed with methanol, the next
stage of purification may not be very good. Thus the general extraction method
for alkaloids is quite possibly not applicable here. That is why I want to have a
look at exactly what the original method was, although the journal seems obscure
to say the least. Another day in the Chem Abs section, I fear.

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Subject: Re: LSA

>Yup.  In a nutshell, you mix the HWBR powder in a nonpolar solvent, keep the
>resultant gunk(I) and throw away the solution.  Then dissolve the gunk(I)
>into a polar solvent, throw away the new gunk(II) and evaporate the solution.
>The final gunk (III) that comes out of the solution has LSA in it. 
>
> gunk(I) = gunk(II) + gunk(III)
> gunk(III) is the good stuff
> gunk(II) is not
> gunk(I+III) are therefore kept
>
>nonpolar solvent = petroleum ether
>polar solvent = alcohol (methanol is better, but is a smidgin poisinous
>  so you've got to be damn sure its all evaporated).


OR

(E.W. Hand) writes :
>Does anyone know about the validity of extracting lysergic acid
>from Hawaiian Wood Rose seeds or Morning Glory seeds.  According
>to the Anarchists Cookbook, althought many on this news group
>seem to question the A.C., you can through a simple process.

K. Lewis responded :
1.  HBWR and MG seeds don't contain lysergic acid, they contain various
amides of lysergic acid (but not di-ethyl amide).

2.  It can be done.  I wouldn't trust the A.C. method, though.  It purports to be
a method for converting the stuff into LSD, which it is clearly not.  Although
LSD is ~100 times as potent as LSAs, the recommended A.C. dosage
_after_ conversion is nearly double the alt.drugs FAQ recommended dosage.
This indicates it's probably a simple extraction which is 50% efficient.

3.  If your purpose is to ingest LSAs, you might as well eat (or grind and
stick up your butt or chew) the seeds themselves.  If you are going to use
it as an LSD precursor, most chemists recommend ergot instead. 

That said, here's an old article I saved on extraction.


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EXTRACTION:

The method I use is a general one - I copied it from one used by some scientists to extract mescaline from peyote, but I have since seen close variations used on many plants. This procedure is followed, whenever a plant is studied for its alkaloids.

A few ingredients and bits of equipment are necessary. I am a chemist, and have my own chemistry set. I have considered manufacture, but I find that there are enough interesting things to do just extracting natural compounds, which is much easier, indeed, possible in the home.


You will need:

A few flasks, glass containers, etc. of suitable sizes, depending on how large a volume you are playing with.
A separating funnel is almost essential - this could be tricky to get without a little effort. If you don't know, it is an inverted conical flask with a hole at the top to pour stuff in , and a tap at the bottom to let the stuff out accurately . It is used for separating immiscible layers.
A vacuum filtration apparatus would be very useful; I did have a bodgy one rigged up myself, but it was always difficult to use. Some kind of still, though, is pretty important to have, although conceivably for a once off you could get by without it, if you don't mind breathing in a lot of solvent.
As far as still goes it is to recover solvent, and leave goodness as a residue at the bottom. I use a bit of quickfit I nicked: a round bottom flask, short column, thermometer on top, and a small condenser... takes for ever, but don't expect to follow this procedure in anything under a day.


Other bits and pieces:

A filtre of some sort is a necessity; preferably a good one, with a vacuum pump if you are filtring gluggy stuff (cactus is the worst, sticky goo, e.g., other things like seeds and bark are better). People have been known to use such devices as coffee filtres, t-shirts, tins with holes in the bottom (as a filtre press) and so on. Whatever you can scrounge. A lab buchner funnel, sidearm flask, and venturi pump are ideal. All this stuff is standard in any chemical lab, regardless of discipline.

Chemicals necessary:

The paydirt (obviously)
Some solvents: methanol (lots), and a non polar solvent. Some people use ether - this is dangerous and doesn't dissolve everything. Your best bet is probably something chlorinated - I use dichloromethane, although chloroform will do (don't breath too much - it is fun at first, but ends up making you feel ill). Drycleaning fluid... petrol.... I don't know what you have access to.
Dichloromethane is good because it is non-toxic, volatile, and a good solvent. [Erowid Note: Dichloromethane was formerly thought to be very safe, but has been shown to be highly carcinogenic and toxic. Scorecard.org. May 2005] It has a major drawback: separation is often very difficult once you have placed your gluggy plant muck in there. The shot is to use large quantities of everything, and be patient.
You will also need an acid (Hydrogen chloride is good) and a base/alkali (Sodium hydroxide is good - that way, if you stuff up, you end up synthesizing salt instead of something nasty.)
Also useful: acid/base indicator paper, boiling chips (porcelain grains) and activated charcoal - see local chemist.

The idea is this:

Most fun compounds (the only exception is maybe THC, and alcohol if you count that) are basic - they contain nitrogen.

So: in general, if you react them with hydrochloric acid, the form a water soluble chloride. If you react them with dilute base in the aqueous phase, they go back to being a base, which is insoluble in water, but soluble in organic non-polar solvents (like CH2Cl2). So, the theory is, that only a base will go from water to solvent and back to water etc. when changed from acidic to basic and back to acidic. This gives you a way of removing all the other crap which is not alkaloid from a sample. That is the theory. When I do this, if I can get down to some brown or green sludge that I can throw down or smoke, I am happy with a good days work. Ideally, you should end up with lovely white crystals, but I think that would require a lot of time and effort, and indeed a considerable loss of product in the process.


Procedure:

Get your stuff.
Dry it as much as possible - this makes life easier later on. You will never get all the water out, but too bad.
Chop it up as fine as possible: a blender comes in handy. You may wish to chop then dry. A word of caution : try to avoid exposing your stuff to excessive heat. I dry in low heat oven. Heat and air destroy good compounds from upwards of 100 degs C. All this bit will depend on exactly what you are extracting.
Once it is finely divided - powdered if possible, put it in a big container, and cover it with methanol. Alternatives to methanol here are ethanol (not as good) and acetone (good solvent - rips the crap out of anything, but is more reactive - can react with your actives).

Now, depending on what your stuff is, you have to let the methanol have time to remove it all. This is best done by leaving in a quiet warm place for a few days, even up to a week, and shaking it occasionally so it is mixed. Some papers recommend solvent extraction (soxhlet apparatus) and refluxing at the boiling point of the methanol (80 degs or so - I can't remember). I usually just rely on time to get the good stuff out.

When you are ready (early in the morning), filtre the muck, to give you methanol+dissolved brown gunk, and a residue soaked with methanol. The residue still contains a lot of good stuff, so soak again for an hour, and repeat, and do a third time if you are feeling generous (3 is the magic number in extraction work).

When you are done, there is another thing you can do finally, if desired: depending on what your stuff is, mix it up with dilute hydrochloric acid, 1M is appropriate. let stand for an hour, then filtre (this may be very difficult) That will get the last of the alkaloids out of the substrate.

You now have a methanol-plant stuff mixture, and a dilute HCL-plant stuff mixture, if you bothered to do that part.

Evaporate the methanol, to leave a small amount of goo. This will contain water, a bit of methanol, and all kinds of resins and muck, and if you are lucky, the alkaloids.

If a very quick and crude extraction was all that was desired, then after stripping the last of the methanol with vacuum if possible, this residue could be smoked eaten or whathaveyou. I leave that to your discretion. However, if a cleaner product is desired, the double layer extraction will need to be performed.

Combine the evaporated methanol gunge with the hydrochloric acid filtrate if you have any. If you don't then mix the methanol stuff with an excess of dilute (1M) HCl. Feel free to filtre again at this point. Anything of marginal solubility here is no good to you. Get the stuff as clean as possible. Boiling with activated charcoal is another useful trick for removing gunge. Just boil it up, and filter off the charcoal for a cleaner brew.

You should now have an acid aqueous solution of alkaloids and water solubles from the plant.

Take your acidic solution, and bassify. This is done by mixing in dilute sodium hydroxide (I use up to 5M to save on total volume. Be careful with conc NaOH - apart from eating skin, it eats alkaloids) As you mix in the NaOH, you will see swirls of white precipitate form and redissolve. Continue until the white swirls stay, and until the solution is quite cloudy. Indicator paper is necessary to see that the solution is basic. If you can't get indicator paper, you can make an indicator by boiling up some purple flowers. The dyes in most flowers go bright red in acid, and green in strong alkali. Just a drop of dye and a drop of mixture should tell you what is acid or base.

The white precipitate is the alkaloids. The more the better.

Next, add equal volume of non-polar solvent (dichloromethane) to the mix. Place in separating funnel, and shake. Separate. This may be very difficult or slow. Adding more solvent, more basic water, etc. may help. Adding lots of salt to the water layer will help break an emulsion. Ideally you want it do this step 3 times - to extract as much as possible from the water layer into the organic. I find this part very difficult, and you have to accept that you will lose quite a lot of material here. It is, however probably easier with some plants that others: cactus is very difficult, barks and seeds would be easier. Use plenty of salt, and agitate to separate. When you have finished extraction, chuck the basic water layer. The solvent layer is kept, and can be backwashed with salty water for a cleaner mixture.

The solvent can now be dried, (using salt or some dry powder, the filtred) (I don't usually bother with this - the old hairdryer at the end can remove some last solvent and water) then strip the solvent in a vacuum to get your final product - some kind of syrup could be expected. This is super concentrated, but may only be half the strength of the original. e.g. put in enough for 10 doses of morning glory seeds, get back 5 doses or more of concentrated alkaloids.

If it is desired to take the process still further, you can do the obvious thing - mix your solvent layer with dilute acid again and extract back into water. Acid layer could be evaporated under vacuum to give salts of alkaloids. Alternatively, if the organic layer were scrupulously dry, bases could be salted out with some organic acid - a tartrate, oxalate could be formed. I have never bothered with such things - you would need a lot of pure extract to be bothered.

The acid-base extraction process can be continued as many times as is desired.

If a truly pure product is desired, the only way to go from here is chromatography. I have never used this at home, and wouldn't think it was worth the trouble, but there will be papers available on what was used for a particular extraction case.



Part 2

Then take that LSA and other amides and do this:

LSD-25 Synthesis from "Psychedelic Guide to the Preparation of the Eucharist"
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 #1

Step I. Use Yellow light
Place one volume of powdered ergot alkaloid material in a tiny roundbottom flask and add two volumes of anhydrous hydrazine. An alternate procedure uses a sealed tube in which the reagents are heated at 112 C. The mixture is refluxed (or heated) for 30 minutes. Add 1.5 volumes of H2O and boil 15 minutes. On cooling in the refrigerator, isolysergic acid hydrazide is crystallised.

Step II. Use Red light
Chill all reagents and have ice handy. Dissolve 2.82 g hydrazine rapidly in 100 ml 0.1 N ice-cold HCl using an ice bath to keep the reaction vessel at 0 C. 100 ml ice-cold 0.1 N NaNO2 is added and after 2 to 3 minutes vigorous stirring, 130 ml more HCl is added dropwise with vigorous stirring again in an ice bath. After 5 minutes, neutralise the solution with NaHCO3 saturated sol. and extract with ether. Remove the aqueous solution and try to dissolve the gummy substance in ether. Adjust the ether solution by adding 3 g diethylamine per 300 ml ether extract. Allow to stand in the dark, gradually warming up to 20 C over a period of 24 hours. Evaporate in vacuum and treat as indicated in the purification section for conversion of iso-lysergic amides to lysergic acid amides.

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.

Preparation #3
This procedure gives good yield and is very fast with little iso-lysergic acid being formed (its effect are mildly unpleasant). However, the stoichometry must be exact or yields will drop.

Step I. Use White light
Sulfur trioxide is produced in anhydrous state by carefully decomposing anhydrous ferric sulfate at approximately 480 C. Store under anhydrous conditions.

Step II. Use White light
A carefully dried 22 litre RB flask fitted with an ice bath, condenser, dropping funnel and mechanical stirrer is charged with 10 to 11 litres of dimethylformamide (freshly distilled under reduced pressure). The condenser and dropping funnel are both protected against atmospheric moisture. 2 lb of sulfur trioxide (Sulfan B) are introduced dropwise, very cautiously stirring, during 4 to 5 hours. The temperature is kept at 0-5 C throughout the addition. After the addition is complete, the mixture is stirred for 1-2 hours until some separated, crystalline sulfur trioxide-dimethylformamide complex has dissolved. The reagent is transferred to an air- tight automatic pipette for convenient dispensing, and kept in the cold. Although the reagent, which is colourless, may change from yellow to red, its efficiency remains unimpaired for three to four months in cold storage. An aliquot is dissolved in water and titrated with standard NaOH to a phenolphthalein end point.

Step III. Use Red light
A solution of 7.15 g of d-lysergic acid mono hydrate (25 mmol) and 1.06 g of lithium hydroxide hydrate (25 mmol) in 200 ml of MeOH is prepared. The solvent is distilled on the steam bath under reduced pressure. the residue of glass-like lithium lysergate is dissolved in 400 ml of anhydrous dimethyl formamide. From this solution about 200 ml of the dimethyl formamide is distilled off at 15 ml pressure through a 12 inch helices packed column. the resulting anhydrous solution of lithium lysergate left behind is cooled to 0 C and, with stirring, treated rapidly with 500 ml of SO3-DMF solution (1.00 molar). The mixture is stirred in the cold for 10 minutes and then 9.14 g (125.0 mmol) of diethylamine is added. The stirring and cooling are continued for 10 minutes longer, when 400 ml of water is added to decompose the reaction complex. After mixing thoroughly, 200 ml of saturated aqueous saline solution is added. The amide product is isolated by repeated extraction with 500 ml portions of ethylene dichloride. the combined extract is dried and then concentrated to a syrup under reduced pressure. Do not heat up the syrup during concentration. the LSD may crystallise out, but the crystals and the mother liquor may be chromatographed according to the instructions on purification.

Purification of LSD-25
The material obtained by any of these three preparations may contain both lysergic acid and iso-lysergic acid amides. Preparation #1 contains mostly iso-lysergic diethylamide and must be converted prior to separation. For this material, go to Step II first.

Step I
Use darkroom and follow with a long wave UV The material is dissolved in a 3:1 mixture of benzene and chloroform. Pack the chromatography column with a slurry of basic alumina in benzene so that a 1 inch column is six inches long. Drain the solvent to the top of the alumina column and carefully add an aliquot of the LSD-solvent solution containing 50 ml of solvent and 1 g LSD. Run this through the column, following the fastest moving fluorescent band. After it has been collected, strip the remaining material from the column by washing with MeOH. Use the UV light sparingly to prevent excessive damage to the compounds. Evaporate the second fraction in vacuo and set aside for Step II. The fraction containing the pure LSD is concentrated in vacuo and the syrup will crystallise slowly. This material may be converted to the tartrate by tartaric acid and the LSD tartrate conveniently crystallised. MP 190-196 C.

Step II. Use Red light
Dissolve the residue derived from the methanol stripping of the column in a minimum amount of alcohol. Add twice that volume of 4 N alcoholic KOH solution and allow the mixture to stand at room temperature for several hours. Neutralise with dilute HCl, make slightly basic with NH4OH and extract with chloroform or ethylene dichloride as in preparations #1 or #2. Evaporate in vacuo and chromatograph as in the previous step.

Lysergic acid compounds are unstable to heat, light and oxygen. In any form it helps to add ascorbic acid as an anti- oxidant, keeping the container tightly closed, light-tight with aluminum foil, and in a refrigerator.

Synthesis of d-LSD maleate or tartrate from lysergic acid with POCl3

Ref:

Johnson, Ary, Teiger, Kassel. "Emetic Activity of Reduced Lysergamides." Journal of Medicinal Chemistry. 16(5):532-537. 1973.

Related:

Huang, Marona-Lewicka, Pfaff, Nichols. "Drug Discrimination and Receptor Binding Studies of N-Isopropyl Lysergamide Derivates." Pharmacology, Biochmistry and Behavior. 47(3):667-673, 1994.

Oberlender, Pfaff, Johnson, Huang, Nichols. "Stereoselective LSD-like Activity in d-Lysergic Acid Amides of (R)- and (S)-2-Aminobutane." Journal of Medicinal Chemistry. 35(2):203-211, 1992.

Hoffman-AJ, Nichols. "Synthesis and LSD-like Descriminative Stimulus Properties in a Series of N(6)-alkyl Norlysergic Acid N,N-Diethylamide Derivates." Journal of Medicinal Chemistry. 28:1252-1255, 1985.

NOTE: JMC 35(2):203-211 has some amazing stereoviews of LSD which might interest non-chemists who like to cross their eyes.

Under reduced light (or red light) a stirred solution of 3.15g (11 mmol) of d-lysergic acid monohydrate and 4.45g (99 mmol) of diethylamine was brought to reflux by heating. Heat was removed, and reflux was maintained by the addition of 2ml (3.4g, 22mmol) of phosphorous oxychloride (POCl3) over a 2 minute period. The mixture was then refluxed for an additional 4-5 mins until an amber-colored solution resulted. The solution was brought to room temperature and was washed with 200ml of 1M NH4OH. The CHCl3 solution was dried (MgSO4), filtered, and concentrated under vacuum (not allowing the solution to exceed 40 degrees C). The last traces of the solvent were removed at 2-5 mm. The viscious residue was dissolved in a minimum amount of MeOH and acidified with a freshly prepared 20% solution of maleic acid in MeOH. Crystallization occured spontaneously. The needles were filtered, washed with cold MeOH and air-dried. Yield was 66% after further purification by column chromatography over alumina (Brockman) and elution with 3:1 benzene-chloroform. The chromatography takes appx 8-9 hours. Alternatively, it can be crystallized as the (+)-tartrate from MeOH. After crystallizing from cold MeOH, it is diluted with ethyl acetate, filtered and the the crystals are washed with ethyl acetate.

This procedure also works for primary amines and small dialkyl amines. LSD, however, probably remains the most worthwhile product. Other interesting amines might be the N-ethyl-N-propyl derivative (LEP) and the morpholide (LSM-775). 75ug of the morpholide have been reported to have been as effective as 50ug of d-LSD but with 45 min onset (vs 1 hour) and a 1 hour peak (vs 4 hours). The procedure would probably work well for LEP, but yields would be reduced for the morpholide. Other N(20)-alkyl-lysergic acid derivatives tend to be more than 10 times less potent than LSD if not effectively inactive. N(6)-ethyl- (and -allyl- and -propyl-) derivates of LSD may be more active than LSD itself, but synthetic routes to these chemicals presently start with LSD and yields would probably inhibit their appearance on the illicit market. (N(6) is the other nitrogen on the ring structure in addition to the N(1) pyrrole/indole nitrogen). Derivatives of LSD (besides LSA/LA-111 and lysergic acid) are not scheduled, but would be prosecutable under the designer drugs act after testimony from a DEA agent that _in their opinion_ the defendant was planning to distribute them.

JohnSanders

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Re: LSD from HBWR
« Reply #3 on: December 04, 2009, 01:03:09 AM »
For the longest time I saw this as the only way to make LSD...Though its not really worth it.

In order to get anywhere around the amount of LSD worth making (10+grams) you'd need around 50,000 HBWR. The cheapest I found was 11,000 seeds for 500 dollars.

Assuming you found the right way to extract them (Uncle Fester's seems to be the most logical) you'd have over 20 pounds of seeds to grind up and extract. 50,000 seeds. Thats a lot of seeds for 10 grams of LSA. Which would be 2 grams of LSD assuming you got a 20% yield.

If you look into it further you can see that its really not .25% per seed, its 25% of all alkoilds in the seeds.

"Alkaloid content of Hawaiian Baby Woodrose seeds

Ergine               22.68   0.136
Isoergine            31.36   0.188
Ergometrine            8.20   0.049
Lysergic alpha-OH-ethylamide      5.79   0.035
Isolysergic alpha-OH-ethylamide      3.98   0.024
The first number is the percentage of total alkaloid content and the second is percentage of dry weight."

So each seed has .136 percent ergine/weight. So...

1 kilo of seeds... is 136mg of ergine, assuming perfect extraction with no impurites. Times this by 5 kilos and you have 500mg. So even my 50,000 seeds assumption isn't close.

Its just not possible.

A more simpler route is something such as ergocristine (what pickard used) bromocristine (remove the bromo then convert) Paspalic acid, ergotamine, and some other ergot chemicals that are much harder to convert..

Personally I've lost all hope to make LSD

Naf1

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Re: LSD from HBWR
« Reply #4 on: December 05, 2009, 01:20:06 AM »

jon

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Re: LSD from HBWR
« Reply #5 on: December 05, 2009, 09:10:12 PM »
dude just pm me for ergotmanine sources speaking to you german why you gotta make it hard???

quetzalcoatl

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Re: LSD from HBWR
« Reply #6 on: December 06, 2009, 03:48:01 AM »
10g of LSD is 50,000 (200 microgram) hits. What the fuck are you gonna do with 50,000 hits?

You need 1g of LSD, tops.  So, LSD from LSA is still feasible.

Although I would like to indicate some problems:

* HBWR Contain clavine alkaloids which will also be extracted, and then mess up the reactions you gave, due to their lack of a carboxyl group. Morning glories are a much purer source of ergine, but the trade off is less overall alkaloid content. (they still contain clavine alkaloids.)

* hydrazine - rocket fuel, watched, poisonous, explosive.
* sulfur trioxide - precursor to sulphuric acid, reacts with water
* lithium hydroxide hydrate
* acetonitrile
* dimethylformamide

All of the above are not simple to obtain.

Good luck to you however, brother. I wish you the best and I hope you are successful.
look on the bright side, if you manage to synthesize even just a gram of LSD;
even slightly impure, thats still 5000 hits (200 mics)  -  a lifetime supply for you and
 your friends.

shroomedalice

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Re: LSD from HBWR
« Reply #7 on: December 06, 2009, 04:10:56 AM »
your going to have to chromatograph any thing comming off a plant for an acid synth.

your products have to be very very pure and extreamly dry.

I would hate to try from natural products unless I had a good source of ergot (ie the high yeilding purpurea types)
and these are very hard to get as they are locked down to my knowlage.

I would love to be wrong as the fungus if you have the right kind would be a great way to go (yes I know about
the black fingers and toes)

I have found a bit of rye fungus but it was no were near good enough for synthesis.

quetzalcoatl

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Re: LSD from HBWR
« Reply #8 on: December 06, 2009, 04:47:39 AM »
Truth there.

Im sure throwing a little chromatography onto the budding acid chemist's 'to-do' list won't set him back
more than a day.

If chromatography was used to seperate the alkaloids, then HBWR could indeed be used, since they yeild
a higher overall alkaloid content.

Ergot is illegal because of ergotism, burning in the extremeties, gangrene and death, as you mentioned;
but I'd like to relay some information, that c. purpurea doesn't always produce alkaloids, and depends on
a cool spring and a hot summer (iirc).

Somone already mentioned the other strain of claviceps but that is equally difficult to obtain.

Some people just won't give up though, They'll end up making LSD come hell or high water...
resourcefulness and sheer determination are the staples of many a good clandestine chemist.


German

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Re: LSD from HBWR
« Reply #9 on: December 06, 2009, 06:06:27 PM »
Some people just won't give up though, They'll end up making LSD come hell or high water...
resourcefulness and sheer determination are the staples of many a good clandestine chemist.

That's actually the only reason I carry my weight around here. I don't know chemistry and am not able to contribute from that perspective, but I can fucking read and follow directions just fine and as a result I can get things going just because I really really fucking want to despite my lack of knowledge (yeah I know, a disaster waiting to happen lol).

I've reserved myself to just buying erogtamine tartrate. This is a very very viable way for someone only interested in personal use amounts like myself. A box of 100 pills of Cafergot with a total of 100mg of ergotamine tartrate in them (100 pills times 1mg each) costs $60. With that 100mg of ergotamine extracted from them (not sure how to do yet) you can get 30mg LSD. With that 30mg LSD you can get yourself 300 doses. Now what in the world does one need more then 300 doses for if he is not interested in selling??? You can make a lifetime's supply off of one $60 box of Cafergot!
« Last Edit: December 06, 2009, 06:08:47 PM by German »

Naf1

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Re: LSD from HBWR
« Reply #10 on: December 06, 2009, 09:13:22 PM »
CafErgot S = suppositories that are twice as strong (2mg) IIRC.

quetzalcoatl

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Re: LSD from HBWR
« Reply #11 on: December 06, 2009, 10:53:07 PM »
I think if one should manage to come by sulphur trioxide, or hydrazine, etc
then it would be a waste to only use 100mg. It'd be best to run your hbwr
alkaloids and work on a gram.  :)

German

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Re: LSD from HBWR
« Reply #12 on: December 06, 2009, 11:13:17 PM »
I think if one should manage to come by sulphur trioxide, or hydrazine, etc
then it would be a waste to only use 100mg. It'd be best to run your hbwr
alkaloids and work on a gram.  :)

I just quickly sourced those and it wouldn't be a problem, but the erogtamine method requires none of those or anything at all difficult to obtain. Taken from Tihkal:

SYNTHESIS : A solution of 6.7 g KOH in 100 mL H2O, under an inert atmosphere and magnetically stirred, was brought to 75 °C, and 10 g ergotamine tartrate (ET) added. The reaction mixture turned yellow as the ergotamine went into solution over the course of 1 h. The stirring was continued for an additional 3 h. The reaction mixture was cooled to about 10 °C with an external ice bath, and acidified to a pH of about 3.0 by the dropwise addition of 2.5 N H2SO4. White solids started to appear early in the neutralization; approximately 60 mL of sulfuric acid was required. The reaction mixture was cooled overnight, the solids removed by filtration, and the filter cake washed with 10 mL Et2O. The dry solids were transferred to a beaker, suspended in 50 mL 15 % ammonia in anhydrous ethanol, stirred for 1 h, and separated by decantation. This extraction was repeated, and the original decantation and the second extract combined and filtered to remove a few hundred milligrams of unwanted solids. The clear filtrate was stripped of solvent under vacuum, the residual solids dissolved in 50 mL of 1% aqueous ammonia, and this solution was acidified as before with 2.5 N H2SO4. The precipitated solids were removed by filtration and washed with Et2O until free of color. After drying under vacuum to a constant weight, there was obtained 3.5 g of d-lysergic acid hydrate, which should be stored in a dark, sealed container.

A suspension of 3.15 g d-lysergic acid hydrate and 7.1 g of diethylamine in 150 mL CHCl3 was brought to reflux with stirring. With the external heating removed, there was added 3.4 g POCl3 over the course of 2 min, at a rate sufficient to maintain refluxing conditions. The mixture was held at reflux for an additional 5 min, at which point everything had gone into solution. After returning to room temperature, the solution was added to 200 mL of 1 N NH4OH. The phases were separated, the organic phase dried over anhydrous MgSO4, filtered, and the solvent removed under vacuum. The residue was chromatographed over alumina with elution employing a 3:1 C6H6/CHCl3 mixture, and the collected fraction stripped of solvent under hard vacuum to a constant weight. This free-base solid can be recrystallized from benzene to give white crystals with a melting point of 87-92 °C. IR (in cm-1): 750, 776, 850, 937 and 996, with the carbonyl at 1631. The mass spectrum of the free base has a strong parent peak at mass 323, with sizable fragments at masses of 181, 196, 207 and 221.

This base was dissolved in warm, dry MeOH, using 4 mL per g of product. There was then added dry d-tartaric acid (0.232 g per g of LSD base), and the clear warm solution treated with Et2O dropwise until the cloudiness did not dispel on continued stirring. This opaqueness set to a fine crystalline suspension (this is achieved more quickly with seeding) and the solution allowed to crystallize overnight in the refrigerator. Ambient light should be severely restricted during these procedures. The product was removed by filtration, washed sparingly with cold methanol, with a cold 1:1 MeOH/Et2O mixture, and then dried to constant weight. The white crystalline product was lysergic acid diethylamide tartrate with two molecules of methanol of crystallization, with a mp of about 200 °C with decomposition, and weighed 3.11 g (66%). Repeated recrystallizations from methanol produced a product that became progressively less soluble, and eventually virtually insoluble, as the purity increased. A totally pure salt, when dry and when shaken in the dark, will emit small flashes of white light.

JohnSanders

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Re: LSD from HBWR
« Reply #13 on: December 07, 2009, 12:44:01 AM »
POCl3 is hard to get I believe, so this is another issue with Shulgins method. Though its much easier than ET.


Naf1

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Re: LSD from HBWR
« Reply #14 on: December 07, 2009, 02:13:55 AM »
Hydrolysis to the parent carboxylic acid, then Hardisons peptide coupling route would be the most user friendly procedure (IMHO).

quetzalcoatl

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Re: LSD from HBWR
« Reply #15 on: December 07, 2009, 12:40:48 PM »
I agree, although I was unsure about the legality of purchasing PyBOP.
I guess since it couples any random amines that it isn't particularly suspicious.
but buying chemical reagents is something that SWIM still remains very
cautious of, despite the rantings of some members on here.

Also, Is it a one-shot thing, or can the PyBOP be re-used?

PyBOP information:
http://chemicalland21.com/lifescience/phar/PyBOP.htm

micro

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Re: LSD from HBWR
« Reply #16 on: December 07, 2009, 04:12:44 PM »
There is a rahter long thread of this subject (well, partially, it is about extraction mainly) Zoklet.nets's Flasks and Beakers forum.

http://zoklet.net/bbs/showthread.php?s=df4e09ec1ea9b1c5f604ab338134f3c6&t=14328

quetzalcoatl

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Re: LSD from HBWR
« Reply #17 on: December 07, 2009, 04:35:14 PM »
OK, thats great. Thanks very much. Moving on..

shroomedalice

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Re: LSD from HBWR
« Reply #18 on: December 08, 2009, 07:49:15 AM »
http://en.wikipedia.org/wiki/Theodor_Curtius

wont work on simple amides like LSA though I belive.

I personaly would want to work with more than a gram the first few times as well or
you might find you loose it all to machanical loss.

smaller volumes are easier if you have the chromatography down as they are solvated there
for making for bigger liquid volumes to work with.

crystalisation and epimerisation would be a hell of a job on a 30mg run.

read otto snows books on lsd in the library here.
well worth the read.

be very very carefull working with any of the reagents needed for this.

POCl3
hydrazine
and SO3

are not to be used unless you have years under your belt if you ask me.

why dont you think the synth is just being given out by people and there are quite a few who do make
it to my knowlage.

one if every one had it in an open forum then kiss the shit goodbye as its number one on the bad lists
for the DEA

two if every one tried it probably 90% would kill them selves and thouse near  to them.

becarefull but by all means if you can work it out and put the time and money into doing it safely dont
let me stop you just shut your mouth when you get it right.


a note on doseage :)

truly if your to be an acid cat the print is a must as is belived by most of the acid comunity.
it gives the cat an idea of what acid can do to some one and hopfully makes them honorable and
reponsible in its use/missuse
acid can be very very dangerous if in the wrong hands.

prints are in the reagon of 1mg and up.

once you have been printed forget 100 mics working for you again well not for many many years anyway.

30mg is not as much as it seems and once you have acid watch it disapear to every one you know.

I belive the stuff should not be sold but given away.
but given only to the right people.

some people do not fair well on acid.
« Last Edit: December 08, 2009, 08:10:21 AM by shroomedalice »

61-50-7

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Re: LSD from HBWR
« Reply #19 on: December 16, 2009, 01:27:51 AM »
Pills are quite a bit more expensive than natural sources imo.  Speciosa is available in bulk at $50 a key.  Most people don't like the alkaloid profile for consumption of the plant, but it still has a higher concentration of lsa's than morning glory seeds.  The alkaloid profile is meaningless for synthesis purposes since mild base hydrolysis converts all the alkaloids to the direct precursor anyway. 

Lets say instead of .25-.3% content like Nervosa, Speciosa has a content of .1% of various ergoline compounds.  This is a conservative ratio based on anecdotal evidence.  Thats $50 a gram. 

Convert the crude mixture of ergolines into d-lysergic acid hydrate through mild base hydrolysis and run that through a column. 

Easier said than done, but don't get confused on price.  This is well worth it.  The scale is still small, a 1 gram run requires the same amount of material as a 10g dmt extraction.