The proper way to DISTILL Ephreda?

ChemLab · Sun May 01, 2005 7:01 pm

Any one have a step by step outline on how to perform this? Also the materials required?

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joe_aldehyde · huxleys associate

i don't know if you really mean to distill ephedra. maybe ephedrine. but rather do an extraction on the plant material, that's the simplets procedure. any ordinary a/b extraction of alkaloids applies to the extractino of ephedra. in fact, i just did a very sluggish extraction and still got about 5 grams of Eph. HCl from 100g raw dried plant.

Senfgas · Mon May 30, 2005 7:45 pm

He probably meant steam distillation of the crude herb?

loki · guinea pig

that's a slightly higher yield than is reported in the literature of its alkaloid contents, biggest number i ever saw was 3%. Sounds like a lot of other stuff must be in it as well (maybe NaCl, maybe just the other alkaloids were not counted in the percentages i've read)

joe_aldehyde · huxleys associate

that wouldn't afford anything unless you add lye to it, and then it would still yield a crap mixture of all kinds of plant oils that are in ephedra (they accompanied me throughout my a/b extraction with their pleasant tea smell Smile

the really weird thing was that i accidentally decomposed a part of the extract by heating the HCl salts too much and ended up with a mud-like sludge, but due to my oh-so-great recrystallization experience (i did actually do that for the second time Wink

i still got those 5 grams pure white crystals that were soo dirty in the beginning and i inhaled quite an amount of methanol it seemed - booo! had to drink lots of ethanol that night, and got some chicks, too! I LOVE EPHEDRINE, it's so smooth on the heart and you can still sleep after snorting till you bleed (i didn't).

Senfgas · Mon May 30, 2005 7:58 pm

But you dont need much solvent, only for a/b from the distillate.. Smile

joe_aldehyde · huxleys associate

my skills are actually quite good since i'm a lucky sucker, but even with my great professional fume hood i'd always breathe some methanol (or maybe it was too much acetone, but i was really dizzy after that lab session).

if you want to save on solvent, do it in a soxhlet, that's what i'm doing next. this way i'll easily fit 500g ephedra in 500ml chloroform. and much less hassle than steam distilling the shit. which is gonna yield a bunch of crap anyways, imo. but somebody try it, write it up and post it so we all can gain some knowledge on this one.

Senfgas · Mon May 30, 2005 8:16 pm

So no crap extacrted too when I use chloroform?

joe_aldehyde · huxleys associate

please be more precise!
you will sure end up extracting some of the oils present in the herb with the soxhlet technique, but that is not going to be a major problem since you have to recrystallize your crystals anyways (if you don't like gassing chloroform with HCl, i'm just too lazy to do that). you could give it a shout, i don't know if the stuff that you don't want would co-precipitate on gassing. recrystallization isn't a bad idea anyways because ephedra also has other alkaloids than the eph-something-stimulant type ones, and as far as i can see, they are being removed upon recrystallization from methanol/acetone.

i dissolved all crystals in boiling methanol, let it cool for 20 secs, added a bit of acetone until precipitation started and then rapidly filtered the stuff while still hot.wash with lots of acetone to remove crap, put acetone wash back in methanol, boil off some acetone and repeat Smile

you will get glistening rhombic needles if you do it right, actually it's not that hard, you will sure get the hang of it quickly.

DrugPhreak · Working Bee

Yeah, that yield does seem high. Even the most potent ephedra should only give ~3.75gm of ephedrine from 100gm of (non-standardized) plant material. Did you separate the pseudoephedrine from the ephedrine via their oxalates or sulfates to see what the yield of ephedrine was? Even though ephedrine is extremely soluble in chloroform it will partially form the HCl so other solvents may bee more suitable here.

joe_aldehyde · huxleys associate

well i guess there ought to be a bunch of side alkaloids in my crystallized product (while the plant material which i have is said to have 8% ephedrine, can't be true). since i can't do a mp. right now i won't know.

i didn't form the sulfates since i'm not so comfy with h2so4 eating my base, and i'm too lazy to scrape the base out of my RBF. if you have a nice method, DP, go ahead. would be nice to see how much really is in my additional 400g i got as a present Smile

ah well ok...if the base dissolves in acetone, then i'll wash out my RBF with a weighed amount and then drop about 80% of the calc'd h2so4 in. rest will have to be titrated, yes? so nice to have 0,1M h2so4 here.

as for potency and true stimulant content, i can only quote my bioassay with friends: burns like hell, ouch! as the crystals were really tiny and dissolved on the mucosa very fast AND after about 100mg for each person involved (all a bit PEA-tolerant), there was praise from everyone about the quality of this product.

joe_aldehyde · huxleys associate

ahh crap you peeps are right...i didn't really get 5g of product, bad typo! more like 3 grams. first crop 400mg, second crop 2.56g.
dunno where i came to believe that it was about 5 grams, jeez...didn't wanna exaggerate :/

loki · guinea pig

lol

regarding recrystallisation technique, i think that a method described somewhere else around here, where you start with dry acetone and slowly add dry ipa while mixing until the crude ephedrine HCl is dissolved adequately, probably works to produce a slightly higher grade of purity, and a better yield than going the other way around it is easier to ensure that you don't add excess alcohol in the first place. definitely don't use water or wet solvents for this as ephedrine/pseudoephedrine HCl dissolves about weight for weight with water.

here's the ephedrine and pseudoephedrine salts solubility info:

joe_aldehyde · huxleys associate

send me some oxalic acid and i'll do it ;P not really...but great method for sure!

hmm anyways how do you titrate with oxalic acid and NOT introduce water? thus, if you titrate out of an alcoholic solution, you will first get ephedrine and subsequently pseudoephedrine.

Guest · Tue Jun 14, 2005 2:57 pm

Oxalic acid is sold in most hardware stores,

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