Hello, first of all sorry for my bad English, Ar finally bought some seeds (2,5kg) for 800$ about and he did it like these:

All the procedure was carried without the presence of natural light (used UV light)

- Got the seeds he put the seeds in the sun with a black-coloured cover for aprox. 1 day (bacause there weren't a lot of dry)
- Crushed the seeds into fine powder with a big cooker grinder machine help, until fine powder then for fine powder with a porcelain mortar aid.
- Added about  2 litres of  room temp slightly hot  deionized water (not boiling) and 0,2g d-tartaric acid per alkaloid gram expected (7,5g so 1,5g d-tartaric acid added)  to a stainless steel container with the powdered seeds in, for 3 days with occasionally stirring with a  painter drill  ( mud mixer ) about 2 times a day stirred for 15 minutes aprox.

- After that the solution was filtered with normal filter paper and gravity filtration , got the 2 liters of water,  washed the water
 with a solution of d-tartaric acid, 0,23g again per gram of alkaloids expected, Ar expected aprox. 7,5 so he added 1,73g
aprox. of dextro-tartaric acid, washed with this solution 3 times it must be now aprox. 3 liters ready to distill.

- This distilled under reduced pressure in a big 5 liter RBF in oil bath until 20 ml of water in the big flask, these water contained the ergoamides like ergometrine/ergonovine/ergobasine, LSA/Ergine, LSH (lysergic alpha-hydroxyethylamide) , etc....

Ar is thinking if this extraction is the most correctly and the water contains all the hydrolysable ergoamides possible that are on the 2,5kg seeds (0,3% by weight that's about 7,5g of alkaloids)

He is thinking of performing with this liquid the hydrolysis with KOH under helium atmosphere and then the coupling method or the classic POCl3.

He is in doubt with the washes with d-tartaric, he thinks that he had to be washed with more tartaric not only the tartaric washed

Greetingss and sorry for my bad english again

Yes hi thank you for the welcome, i'm not a chemist only amateur so i don't know a lot of things all i did was extracting the theorical alkaloids on that water, i don't know how to precipitate them so i have them diluted in an black bottle in the refrigerator, my question is how i can crystallize them without damaging the alkaloids, for example evaporating the water can i distill them under reduced pressure or gassing with something to precipitate withouth damaging from light or temperature? any info is very apreciated

Thank you!

Wouldn't a nitrogen atmosphere suffice?

i'm thinking of doing the hydrolysis with a septum , and a 3 neck RBF, in a heating mantle with a variac i think...

i thinking on doing that, one far friend, you know was experimenting and he used helium and nitrogen tanks, dependes on the situation, never used argon.

Thank you amigos!

 Thanks to the OP for sharing this anecdotal report.

  I'd like to comment on a few things mostly related to the extraction method posted. Please feel free to correct and/or elaborate as needed--
 
 -- I do not understand the use of natural heat to dry the seeds prior to extraction when the technique in question employs an aqueous solution.

 -- The reason UV light is employed is because it allows one to visualize the alkaloids in question via their chemoluminescence. It does not protect the compounds in question from harm and will in fact damage them just as sunlight will if they are exposed to it for a prolonged period. On a side note, UV lights are used by collectors of LSD blotter art to render dipped, 'active' sheets inactive and thus kosher for trade and possession free from legal persecution.

 -- It looks like one large extraction was performed and then after filtration the seed powder mush was washed with an additional liter of tartaric water. What made you decide on these amounts of solvent and is there a reason you opted for one large extraction versus several smaller extractions?

 -- Have you performed any sort of quantitative test to determine what kind of concentration of ergot alkaloids you might have in your solution?

 -- Depending on the variety of A. nervosa seed you are working with, both the concentration as well as the profile of alkaloids can differ significantly, and while some of these should hydrolyze (in theory) to LA, there are some such as the clavines which certainly will not. In short, I am doubtful that any full-spectrum extract such as the one you might have will leave you with a utilizable product following the hydrolysis attempt. One would need to purify and isolate the desired ergot alkaloids from the others, either via re-crystallization or preferably running a column, prior to going for the hydrolysis step.


  As for the steps that might hypothetically follow a successful hydrolysis of said alkaloids, that is an entirely separate concern altogether, rife with many caveats and complications in its own right.

  I am curious to see what, and how much of that what your experiment may have yielded, if anything. If you are indeed able to characterize the assumed yield, please do share.


    --Sol

 

UPDATE: I'm thinking to try next month , the good will be kept in refrigerator or freezer with a black cover for not light and in a amber bottle and all this in two or three double-close ziplock ( i'm thinking the freezer because it hasn't got light bulb) will the goods decompose?

Well actually that tech it's not from my friend it's custom made, my ''far'' friend we can say just got the stuff from the OTC pills in some country and make the stuff, he got arrested or killed, i don't know anymore because he just disappeared, the extraction, i think that i have got things, but i'm not going to try this yet, i have it on the refrigerator right know, will try the iodosaf finklestein firstly, i actualized things on you.

thank you in advance and sorry for my bad english