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LSA extract, crystal yielding.

Migrated topic.
director of sound

director of sound

Rising Star
sorry swim dosen't have any pics yet but swim has more HBWR seeds on the way. swim will have to ask the mods first if he can post the whole process or just the process to LSA. swims total process deals with the extraction of LSA for hydrolysis to D-lysergic acid monohydrate and an epimerization process to convert the ISO-lysergamides into active lysergamides. this may be a potential board rule breakage if the whole thing is posted as there is only one use for lysergic acid i know of. though yields are lost to the hydrolysis pure lysergic acid is the result. alternantly you can follow the process up to the step that yields LSA tartarate and stop there.... the proces is a little bit different than a pandoramix or other extractions. the seed powder is first acidified with acidic MeOH (tartaric, maleic or fumaric) and removed by evap or vacuum before extraction with DCM or chloroform (diethyl ether will work too) the NP extract is saved for the epimerzation process as it contains the ISO forms that will not react with the acid in their current state. after the solvents evap with no trace of oils or fats methanol is once again used to extract the seed powder 3 times then evaped down to a small ammount (a few ml mabey 5ml per each expected gram of LSA) diethyl ether is added untill the solution stays cloudy and is then placed in the freezer for crystalization over night. after filtration and drying you will have some quite pure crystaline Lysergic acid amide tartarate. as for the epimerzation the NP solvent is removed by vacuum till a oily residue is obtained. the residue is dissolved in MeOH and a saturated aqueous sodium bicarbonate or sodium carbonate solution is added to the oily residue/ MeOH and extracted with chloroform. the chloroform is dried over dry sodium carbonate and removed by vacuum. that residue is dissolved in a minimum of MeOH and .232g of tartaric acid is added per each gram of LSA freebase. the diethyl ether again is added untill it stays cloudy and crystalized in the freezer for an additional yield. swim will stop here because the processes after this are the road to D-lysergic acid monohydrate. unless a mod says i can post the rest this will remain as is. it is a little more in depth than traditional LSA extractions but yields a crystaline product rather than a yellowish oil... more will be to come when the seeds arrive...
 
this method sounds awesome director:d i would love to see the pics for this when possible. perhaps you should later post a tek with detailed description so that average laymen like myself can understand the process more thoroughly.
I would like to hear the mod's opinions as well, if a further description of this tek is appropriate to post here on Nexus.
 
will do, it should be posted within the month once i get everything togather. yea me too i was wishing the mods would have chimed in on this by now. im just gonna play it safe and cut the tek short of the epimerization and hydrolysis because it gets to a 'synth/precurser' point there.
 
Well, synthesis procedures that are not safe enough for the average chemist and require difficult to procure (but most importantly watched) chemicals are simply not allowed here.

I understand that some people dream (literally) of being able to make lsd, but as long as a safe, BOOM-free and straightforward procedure is devised, nothing will be allowed.

As far as LSA, this is good work and thanks for it, maybe also add some pictures and make the write-up clearer, e.g. bulletpoints and paragraphs? Also, some precautions should be added, e.g LSA and friends do not stay happy in basic solutions so DCM pulls should be swift, light can harm them as well etc. Also a rough idea of starting material and expected yield should be given, no?
 
so in the end are you propsing that the iso converts be turned into LSA again or LSD (the part which u asked permission to post about i mean)??

lsa im guessing which would still technically be synthing?
or u mean LSD which IS synthing?
 
i will merely post a tek to get crystaline LSA what you do with it after that is at your own risk. a short bit of research and you can find out hoe to convert the inactive iso-LSA into active and go beyond that breaking the moleclue down to its basic acid but that would be too much bad juju to post that here. you can find that out on your own.
 
basically the extraction takes into account that the ISO-LSA, ergometrine and elymoclavine that is contained in the seed will not form a tartarate salt or maleate salt. if you were simply to do a methanol extract of the seeds that you would consentrate by vacuum or evap then defat with chloroform you would be left with a residue of freebase LSA which would be dissolved in methanol (4ml/g) and treated with tartaric acid (232mg/g) once it is allowed to react in the dark for one full hour the addition of diethyl ether will force the LSA to crystalize out and any left over trace ammounts of other alkaloids would stay dissolved. if you further that reaction the chloroform 'defat' would also be consentrated down to a residue and dissolved in a consentrated soduim bicarbonate solution which should not atain a ph above 9. that will effectively be an epimerization which would convert the inactive isomer into the active one. the same process would be repeated, ie consentrate, dissolve in MeOH, treat with tartatic acid and crystalize with diethyl ether. as a whole without the epimerization one could hope to get about 600mg (mabey a little more depending on seed alkaloid content) per each kg of seeds extracted. with the epimerization one could double that ammount. if you choose to go past that and hydrolize to D-LA (you should not) your yields will decrease quite alot. 10g will be reduced to a little over 3 so your 1.2g would turn into 350mg or so.
 
Hi director of sound. Any chance you can write up a simple tek for the extraction of LSA from HBWS? Would someone be able to perform it without having an extensive knowledge in chemistry?

You sound very smart btw :)
 
well my source for a few kg of seeds fell through due to a drought in hawaii right now so ill have to wait a little longer to get my hands on some seeds...
 
Good luck my man! I am looking forward to see the outcome, but please show appropriate safety measures as these compounds are very potent and readily absorb through skin and lungs. I am especially looking forward to see if the nearly pure LSA - if the extraction works - will have the effects we expect. It has recently come up a discussion about the truth to visual activity of LSA. It may be that ergometrine is the sole visionary compound.
 
vapors should not be too much of a big deal because the alks will be in solution and a salt form most of the time. as for skin protection nitrile gloves... some of the solvents you may choose for parts of the extraction could eat through natural latex gloves if accidently spilled on them. most of the protection will go twords the alks, protection from air, heat and light will keep them in tightly closed containers (preferably non breakable opaque PTFE bottles) in a cool place. in all accual reality these, though dangerous alkaloids are very easy to work with safely if you practice general chemistry saftey and common sence.
 
SWIM extracted pure LSA (with help from a friend), strychnine, scopolamine, and hyoscyamine before. Talk about dangerous!

Just make sure you have gloves whenever it's possible any might get on your fingers, and goggles if any might splash, and make sure you clean up everything when you're done. The last thing you want is an unnoticed spill of potent alkaloids sitting on the table. Imagine, you don't know its there a few days later and you touch the alkaloids, they soak into your skin, or you rub your eyes, you get the picture.
 
Thanks for the post... SWIM has been working on an LSA extraction for a few weeks now... ~kg of HBWR seeds were washed, crushed, and left in a dark place to soak in naphtha for a few days... The naphtha was then dumped, and this step was repeated three times... The seed mush was then left to soak in ethanol for few days. The ethanol was collected, and run through a vacuum filter. This step, too, was repeated three times. The collected ethanol has been evaporating in pyrex for a few weeks... There are crystals, but there is also a yellowish residue, as well as a brownish film...

A couple of things. First, he's interested in running the LSA through a column. He found one (a column) for really cheap on ebay, but he is not exactly sure how to do this. He was hoping someone might post a simple tek, using widely available solvents, detailing how a column (on lsa) is run... The few things he could find online were either too vague or involved the use of solvents that are too hard to get a hold of without raising eyebrows. What should be used for an eluent and in what proportions? What kind of UV light should be purchased? etc... Some kind of simple 1,2,3 in this regard would be greatly appreciated.

Second, he's very interested in trying to put to rest whether or not Acetaldehyde converts the LSA to LSH... Has anyone come across anything new regarding this debate? I found the following somewhere, which claims Acetaldehyde can be easily synthesized from widely available product:

The simplest way to make acetaldehyde with little byproducts is simple treatment of ethylene glycol (common radiator antifreeze in the USA) with dilute aqueous H2SO4. This is called the Pinacol Rearrangement.

Pinacols are vicinal glycols, meaning 1,2-diols of course.

HO-CH2-CH2-OH + H+ ---> HO-CH2-CH2-OH2+ ---> HO-CH2-C+H2 ---> -O-C+H-CH3 ---> CH3-C(H)=O.

Basically, one alcohol gets protonated, then the dehydrating abilities of H2SO4 remove water, forming a carbocation, which rearranges to the more stable carbocation, which is the one on the carbon with the other hydroxyl, and then the alcohol extrudes a proton (so the protonic acid is a catalyst, not a reactant) and the O-C bond strengthens to a double bond.

The Pinacol Rearrangement is used all the time in clandestine labs, for rearranging 1-phenyl-propan-1,2-diols to 1-phenyl-2-propanones, which are direct precursors for amphetamines and methamphetamines.

The Pinacol rearrangement also works on epoxides because the acid opens the epoxide ring to the diol with the water present.

All that need be done is heat some ethylene glycol and dilute H2SO4 together for awhile. There are nearly zero side reactions. Zero that I know of, but Im covering my ass just in case. :p
Click to expand...

Just a thought. Either way, solutions of Acetaldehyde are available online. He's never done TLC before, but he was thinking that the simple experiment of developing separate LSA and LSA+Acetaldehyde slides could shed some light on this topic, no? What do you guys think?
 
does anyone have info about alkaloid content in leaves on certain species like morning glory and hbwr... just wondering if there is any use for the leaves and or flowers..

paz
 
the leaves do have some alks but not alot. somewhere in the area of 30-100ug per 100g leaf... not worth it. as for chromatography you want basic alumina or silica (not acidic) use benzene and chloroform as the elutant (1:3) and follow the blue band with a weak long wave UV light (use spairingly as it destroys your product). same as isolating LSD freebase by chromatography. ad for loading the column thats a bit of an art. make a slury with the elutant and the alumina/silica and pour into the column and let it settle with no bubbles or cracks. cap the media with about 1/4 to 1/2 of regular sand and drain out the elutant till only about 1/8 inch remains above the bed of sand/media. dissolve the freebase (you have to base what you got with either ammonia or sodium bicarbonate and extract with chloroform and dry/remove the chloroform th get the freebase residue just dont let it get above ph 8.5 or it will change it into ISO-LSA) in a minimum of the elutant and add to the column. open the valve and let it progress through adding more elutant as the fluid level gets close to the media. the fastest moving blue band is the LSA and the smaller (or larger) one behind it is ISO-LSA and other clavine alkaloids.
 
Director, you sound like you know what you're doing!, do you have any thoughts on the LSH stuff? Your name is "director of sound," hypothetically speaking, what substance do you think is best to aid in musical inspiration and creativity? Anyways, chloroform is kind of expensive and must be ordered from a chem supply place, does ordering something like that raise eyebrows?
 
I edited the information so far to make it a bit more readable and understandable.

Let me know if there are any mistakes and if you have any additions please submit them!

I also attached the raw TeX file if anybody is interested in editing and building it themselves.

(You can make a patch file with the program 'diff' and I will merge changes using 'patch')

diff -u TheOriginalFile.tex TheNewFile.tex > UpdateSubmission.patch
 

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