director of sound
Rising Star
here ya go... sneak peak on a new tek im working that beats manske outa the water. it will be posted soon.
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ultra pure harmaline fumarate!
- Thread starter director of sound
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director of sound
Rising Star
yea its taking forever for my consentrated acetate salts to evap. cant go on to the next step untill i get them dry. ptrobally gonna throw a little heat on them with the fan and see if i can get it done overnight. its just so god dang humid where im at. anyway here is what they look like dry and out of the jar....
director of sound
Rising Star
69ron said:
quite strong. it took more poking than i thought it would to knock the clusters loose. i was afraid of crushing them up at first but when i poked at them they were very solid and allmost glass like. id say they are a good deal stronger than the HCL crystals. it is also not as bitter as other salts i have tasted (citric, acetate, hydrochloride) a bit more tolerable. as for sublingual absorbtion i can start to feel the 'warmth' and the first effects in about 10 min. i take a tincture of them at night to enhance dreams. the solution was 500mg in 15ml distilled water, effectivly the mother liquor those crystals grew from when evaped.i take 5 drops. it seems the bioavailability of this salt is much higher than the other salts as the dose i was taking would be close to 25mg with effects felt.
Beautiful crystals! Looking forward for more information on that.
Manske is indeed a laborious process but the great advantage of it (and only reason its still used before base-precipitating, AFAIK) is that it separates harmalas from vasicine and vasicinone. How do you know that those alkaloids are not present in your tek?
In any case, even if there is no guarantee those unwanted alkaloids were removed, if the process you are doing makes filtering easier , then one could easily just salt-precipitate afterwards once (without all the oils that make filtering so difficult in the first manskes), and then crystalize again the fumarates the way you are doing or precipitate the base if one wants.
One more question, why do you say 'harmaline fumarate' and not harmine? Was it removed for some reason, or it doesnt precipitate as well, or maybe this is just part of your experiment and the harmine also works?
Please do share with us what process you have been doing, im curious as I was thinking of doing another rue extraction soon
edit: by the way, I hope you dont mind but I edited the name of the thread, its fumarate, not fumerate
Manske is indeed a laborious process but the great advantage of it (and only reason its still used before base-precipitating, AFAIK) is that it separates harmalas from vasicine and vasicinone. How do you know that those alkaloids are not present in your tek?
In any case, even if there is no guarantee those unwanted alkaloids were removed, if the process you are doing makes filtering easier , then one could easily just salt-precipitate afterwards once (without all the oils that make filtering so difficult in the first manskes), and then crystalize again the fumarates the way you are doing or precipitate the base if one wants.
One more question, why do you say 'harmaline fumarate' and not harmine? Was it removed for some reason, or it doesnt precipitate as well, or maybe this is just part of your experiment and the harmine also works?
Please do share with us what process you have been doing, im curious as I was thinking of doing another rue extraction soon
edit: by the way, I hope you dont mind but I edited the name of the thread, its fumarate, not fumerate
So the title of this thread is "ultra pure harmaline fumarate" yet I see no proof of purity or reference to it. Did I miss something?
Btw, those are some cool looking crystals.
Btw, those are some cool looking crystals.
director of sound
Rising Star
my process is in no way easier to filter and is quite laborous but gets real good results and yields. as for the no harmine, part of the process includes a partial to full hydrolysis of harmine into harmaline via heating in an alcoholic solution of acetic acid leaving behind only a small percentage of harmine around .5-1%, the rue seeds only have about 6% harmine out of the total alkaloidal content of 5-9% dry weight. the process starts like manske but uses the alcoholic acetic acid solution for the 3 pulls i do, the harmaline is then base preciped, filtered out and salted with acetic acid and dried. you then dissolve the acetate salt in a solution of 2:5 acetone and water and base it again, the acetone prevents the harmaline from precipitating so it can be extracted away from the byproducts of the previous ectractions with a solvent of 5:2:2 methylene chloride: xylene:toluene. from there it is salted with FASI and several consecutive recrystals with different solvents eliminates traces of byproducts. vasicine and vasicinone do not precip in basic solutions containing an alcohol, their freebase form stays dissolved in the solution, had ad it been an aqueous basic solution with no alcohol some would have preciped. there is a further process past the origional precip and acetate salting/hydrolysis that eliminates the last residual traces of vasicine and vasicinone. as for the purity i do not have GC/MS data but based on the crystal structure formation and the fact that there was no residue other than the crystals left after the final evap i have at least 95%+ pure harmaline. some of the same crystals that were re-based and dried to a constant weight melted at 237*C which is only 3*C higher than pure harmaline, that means there might be a contamination of harmine in the area of 2-4%. if i could find MP data for harmaline fumarate i will conduct another melting point test to see how close it is to pure. if someone knows where i can send a sample to be tested i will send one.
harmala fumarates has a low solubility in water, so you could probably grow nice crystals if you have a solution of harmala fumarates, then let it evaporate in room temperature for days/weeks.
thanks for the extra info. Too bad about not skipping the annoying filtering
From where do you get the .5-1% data of the harmine present, if you didnt analyze it? As for the rue seeds having only 6% harmine, again, how do you know? I ask because I have had several different rue batches with different alkaloid contents. I've had it from 3:1 harmine:harmaline to 1:2 harmine harmaline, but never so little as 6% harmine.
As for the purity, how do you know that vasicine/vasicinone do not precipitate in basic solutions containing alcohol?
Melting point is indeed a good indication of purity but still it would be interesting to have it really analized.
I hope you understand that my questions are not at all because I dont believe you or think you are wrong, but its important that we get the details clear and that we make sure the information is reliable. In any case im happy you are experimenting with different things, this is always interesting, the more knowledge we have on different extraction methods, the better
From where do you get the .5-1% data of the harmine present, if you didnt analyze it? As for the rue seeds having only 6% harmine, again, how do you know? I ask because I have had several different rue batches with different alkaloid contents. I've had it from 3:1 harmine:harmaline to 1:2 harmine harmaline, but never so little as 6% harmine.
As for the purity, how do you know that vasicine/vasicinone do not precipitate in basic solutions containing alcohol?
Melting point is indeed a good indication of purity but still it would be interesting to have it really analized.
I hope you understand that my questions are not at all because I dont believe you or think you are wrong, but its important that we get the details clear and that we make sure the information is reliable. In any case im happy you are experimenting with different things, this is always interesting, the more knowledge we have on different extraction methods, the better
PlainCoil
Rising Star
Weird synchronicity....
SWIM left a large flask containing a difficult rue extraction in his closet. The mixture was of dirty manske'd crystals dissolved in water, and whose freebase would not precipitate as expected when basic water was added (even after several days). This frustrated SWIM, so he added a saturated salt solution and put it in the closet.
Many, many months later, most of the water evaporated, there was a crystal cake on the sides (presumably nacl), and there were HUGE radial crystals that look just like the ones pictured in the OP! Except they have bits of dirt on the needles and possibly still some salt contamination.
He thought this must be some contaminant - a byproduct of the salt and sodium carbonate or something, until he found this thread! He then realized he had huge glass-like shards of ultra-clear harmaline hcl! He fished 'em out with chopsticks and is now drying them on a coffee filter in a silica dessicant chamber.
Any advice on cleaning it up from here? What would be a good route for re-x, 500mg in 15ml DI water as mentioned?
SWIM left a large flask containing a difficult rue extraction in his closet. The mixture was of dirty manske'd crystals dissolved in water, and whose freebase would not precipitate as expected when basic water was added (even after several days). This frustrated SWIM, so he added a saturated salt solution and put it in the closet.
Many, many months later, most of the water evaporated, there was a crystal cake on the sides (presumably nacl), and there were HUGE radial crystals that look just like the ones pictured in the OP! Except they have bits of dirt on the needles and possibly still some salt contamination.
He thought this must be some contaminant - a byproduct of the salt and sodium carbonate or something, until he found this thread! He then realized he had huge glass-like shards of ultra-clear harmaline hcl! He fished 'em out with chopsticks and is now drying them on a coffee filter in a silica dessicant chamber.
Any advice on cleaning it up from here? What would be a good route for re-x, 500mg in 15ml DI water as mentioned?
Attachments
director of sound
Rising Star
those are quite impressive plaincoil. probally clean enough as is and in freebase form? you could dissolve in acetone:water (2:5) and extract with methylene chloride or xylene to get rid of any NaCl contam and salt with youre prefered acid for use. i mean to try gassing the dry solvent sometime and see what the results are compaired to the FASI salting i use. i am unsure if the DH2O rex would work on a freebase though, it may need to be turned into a salt first. heating is needed to dissolve all the fumarate in water and left in the small vial i used for about 1.5 weeks to a full rex after filtering out the unused fumaric acid and othe insoluables. data i have found in scientific papers state that out of the total alkaloidal content of rue seeds up to 6% is harmine. i dont doubt that from different areas and climates the content can vary mabey even substrains/speices can play a factor. as i said before i would love to send some off to be tested for purity but i have no idea where to look for that.
kemist
John
ILPT doesn`t like the idea of swiy , using nasty solvents to get harmaline. He also isn`t happy with the fact ,swiy`s tek targeting harmaline only.
ILPT and parrots preffer effects of harmine and using harmaline only occasionaly
Same as endlesness, ILPT`s seeds were always higher in Harmine and he actually tried to increase ammount of harmine by converting of harmaline
ILPT and parrots preffer effects of harmine and using harmaline only occasionaly
Same as endlesness, ILPT`s seeds were always higher in Harmine and he actually tried to increase ammount of harmine by converting of harmaline
69ron
Esteemed member
kemist said:
I agree with the toxic solvents. Why use them? If you can extract without using toxic crap, I think making a new tech that uses toxic crap is a step backwards. There must be a better way to do this.
As for the harmaline versus harmine debate, harmaline is STRONGER. It’s about 2 times stronger than harmine. So you get more bang for your buck from harmaline. Unless you specifically prefer harmine, this is a good thing.
Some people prefer harmaline and dislike harmine. So while I know several on this forum keep saying harmaline is better than harmine, that’s only true for some people. It’s not true for everyone. Just like some people prefer coffee and others prefer tea, some prefer wine, others prefer bear. It’s a personal thing.
SWIM prefers tetrahydroharmine over both of them, by far. In most cases SWIM would never use harmine or harmaline, unless he specifically wants to introduce mind fuck, or if he’s out of THH.
Harmaline is the cheapest of the three and most potent, so SWIM always seems to have that sitting around. It’s nice as a sedative at night. It’s got its own value because of it’s unique sedative effects. It harmonizes well with certain psychedelics. It’s got more “crack your head open” potential than harmine or THH. Sometimes that’s needed for certain mixes.
I know of several people who prefer a mix of THH, harmine and harmaline, and find a mix without harmaline to be lacking in depth.
Anyway, this is a personal thing. If you like one over the other, it doesn’t mean one is better than the other. It just means YOU LIKE IT MORE, and there will always be those who think you are wrong.
director of sound
Rising Star
kemist said:
ive been looking at some older scientific papers on reducing harmaline to THH. much in the same way one would reduce DMT-N-Oxide to DMT using Zn metal and HCL. even what ever harmine present would be reduced to harmaline and in turn to THH given time. still untested. origional outdated methods used HCL and Na metal or HCL and litlium but the higher yielding method with Zn and HCL is presently used. i may try conversion of most of my ending stock of harmaline after testing a small rxn to see the results. as for the solvents yes one could do away with them and possibly use limolene as apposed to DCM xylene or toluene. i just have easier access to those three and know they are pure technical grade without any contams that would show up after the use. in my version they dont get evaped they just pull the desired substance away from the unwanted ones so i get much cleaner end results. infact the used solvents can be reused many times after the initial use and salting. none are present in the end product and the desired ones are only in the solvent for a few minutes or hours at most before they are turned into a salt and therefore removed from the solvent.
kemist
John
ILPT never made any profit from his extraction a solvents swiy mentioned he would use for extracting of other compounds where isn`t possible to use water.
ILPT also got nicely looking crystals (his were hydrochloric salt ) crystalized from solution of vinegar and water, but after drying and converting to freebase the final powder didn`t look perfectly clean.
It depends of the seeds he thinks. Sometimes he`ve done 2-3 manske 1 a/b precip. and 1 pH selective a/b precip. where first seed`s acidic boil weren`t "greasy" like.
With some crappy seeds some other times 6 manske and 4 a/b wasn`t enough to clean it up nicely.
Nevertheless he wanna stay away from toxic solvents
@ 69ron:
ILPT also preffer THH but he doesn`t wanna buy it and didn`t have time to start with his experiments yet
He still wanna to investigate non-mescaline cacti alkaloids and harmine to THH conversion, but last few months he has to do something else. As you can see we havn`t posted much recently.
ILPT also got nicely looking crystals (his were hydrochloric salt ) crystalized from solution of vinegar and water, but after drying and converting to freebase the final powder didn`t look perfectly clean.
It depends of the seeds he thinks. Sometimes he`ve done 2-3 manske 1 a/b precip. and 1 pH selective a/b precip. where first seed`s acidic boil weren`t "greasy" like.
With some crappy seeds some other times 6 manske and 4 a/b wasn`t enough to clean it up nicely.
Nevertheless he wanna stay away from toxic solvents
@ 69ron:
ILPT also preffer THH but he doesn`t wanna buy it and didn`t have time to start with his experiments yet
He still wanna to investigate non-mescaline cacti alkaloids and harmine to THH conversion, but last few months he has to do something else. As you can see we havn`t posted much recently.
plumsmooth
Rising Star
Just curious if their reasons for preferring, or personal subjective effects of all three could be elaborated on.
Thanks...
69ron
Esteemed member
plumsmooth said:
Well B. caapi is mostly a mix of THH, harmine and harmaline, and many people prefer that over rue. SWIM is not really the guy to talk about this because he doesn't really like B. caapi. He prefers rue over B. caapi because B. caapi feels so toxic. The purge is horrid. I don't see why anyone would like that. Besides the toxic effects of the caapi, the mental effects are nicer than rue at larger doses. But rue is also nice at moderate doses, and just as nice as caapi at moderate doses, but without the toxic body feel.
Harmaline has stoning effects that are a little similar to marijuana which the others lack (THH lacks this most of all). Harmaline introduces a little more of a wild side to the experience. Some people find a mix without harmaline is not wild enough. Not adventurous enough, and too stimulating. Harmaline can help calm your nerves a little bit.
For example, THH taken on it's own with DMT produces one of the most amazing psychedelic experiences a person can have (according to SWIM and several others). The trip is full of boundless mental and physical energy. There's no stoning effect. The mind is clear, but the trip goes at such an amazing pace that some people find it overwhelming. Harmaline taken with THH will mute the trip a little. It will turn your energy levels down a little, making the experience slower, and not as supercharged. Some people like that. SWIM doesn't though. Of all the DMT mixes SWIM has tried with different MAOIs, the DMT + THH mix is by far the best there is.
