recrystallization help

[whitebread420]

Sorry for the double post, can a mod delete my other thread in the open discussion?

I performed shaggy's jungle tek and yielded about 10 grams of jungle spice. I smoked it and the least i can say is it works great. so i wanted to try and recrystallize a little bit of it with heptane to produce crystals, and the only thing i got was a red oily substance again. i heated both the heptane and the jungle spic in test tubes in a heat bath. i kept everything hot. i washed about 4 times. the brand of heptane i used was bestine rubber cement thinner. the heat bath was just below boiling, so the heptane was pretty hot. i did not add the heptane until the jungle spice was melted to a dark goo.

i decanted the hot heptane and just squirted it onto a pyrex dish. the solution looked cloudy and yellow/white. so i thought things were going good. so then what i did was gave the dish a swirl to get it all spread out evenly, and that's when the yellow solid seemed to redissolve. i left the dish on the hotplate at low heat with a fan blowing on it (eventually turning off the plate after an hour, with another two hours fan blowing on it), and it never fully dried. i scrapped up half of it and got a red oily substance (that upon agitating with a glass stir rod will turn to a peanut butter like substance) that looks like what i got from the initial extraction. i left the other half alone to see if anything will happen in coming days with the fan still blowing on it. Am i missing something on the technique of recrystallizing? we do this in my orgo lab (final semester in college and just now taking that) so i thought i kinda knew what i was doing, but i guess not. im pretty sure if i just put the solids mentioned before (before i swirled the dish) thru a vacuum filter (which i don't have at home) i would have collected some yellow/white crystals.

thanks for the help

p.s. what i'm hoping to do is grow some neat, flowering crystals. if someone can basically point me in the direction on how to do that, that would be great too.

 

[whitebread420]

k ... i'm basically going to hijack my own thread. im just desperate for some input on how to get a more pure substance, lol.

This is a first time extraction so i thought my own, on going thread would be useful. if not can a mod move it into a sticky thread?

First i'm going to explain what i did.

with 500 g MHRB powder(source of powder: ShamanHerbs is for sale at Squadhelp.com! good deal, got high yields, i would recommend) in 1 gal dH2O with 30 g citric acid, i cooked this mixture in a heat bath (100 C) for 8 hours and occasionally stirred . some of the volume was allowed to reduce. in a large conical shaped wine jug (cleaned very well), i added 200 grams NaOH and 250 ml's of dH2O to make a 200ml 20 M NaOH solution. i swirled it untit the NaOH almost fully dissolved. Then i added the hot MHRB solution to the jug. the solution turned black. there was extra volume at the top of the jug to add about 15 ml's of toluene for extraction. so i put the solvent in there and rolled it around on the ground and stuff for about half an hour, and repeated this four times. by the last pull the solvent was almost clear. i collected the solvent on a large pyrex dish and heated it with a fan on it until all the solvent evaporated. what i was left with was about 10 grams of a red/orange oil .. presumably jungle spice. when i stirred up the oil with a glass stir rod, it turned to a peanut butter like substance, and got harder. it easily starts to melt when you touch it. i smoked this, and it blasted me the hell off, and the come down was very amazing.

so today i took some of it and did what i said above in my first post. so with further research a lot of people suggest freeze precipitating it. the reason i am weary about this because i tried this in the past. I did everything i mentioned in this thread, but what i did is i left the oil on a pyrex dish and put it on ice. this made water condense in the inside ruining the whole god damn thing, wasting about 80 or so dollars. so will a mason jar really remedy this?

another question i have is the best solvent of use for the initial extraction. should i use naptha? i used toluene initially and i suppose this extracts a lot more "stuff". also when freeze precipitating do you put each pull in it's own mason jar? or can you combine them all in one. also do you seal the jar right away as to not let any solvent evaporate?

thanks a lot to any help you all can provide. i know the answer is probably out there, but with chemistry i know better than anyone that even though the theory is very simple behind this stuff, the slightest changes in strategies can make a world of difference. lets just say i'm not that great at this kind of stuff lol. thanks again.

 

[endlessness]

Here's a couple of FAQ links that might be of your interest:

FAQ - DMT Frequently Asked Questions and Troubleshooting Guide - DMT-Nexus Wiki

wiki.dmt-nexus.me

FAQ - DMT Frequently Asked Questions and Troubleshooting Guide - DMT-Nexus Wiki

wiki.dmt-nexus.me

A very impure (red stuff from toluene) wont turn pure white with just one re-x, you might need to do it two or three times.

I dont understand why you lost anything with your freeze precipitation. You dont lose anything until you throw it away. Water condensing in freeze precip container is not an important issue, water will evaporate and your dmt will still be there.

As for using mason jar, i dont really trust the rubber from the inner part, maybe put a layer of alu foil and then close it, as solvent touching it may dissolve some of that rubber/plastic.

Regarding what solvent to use first, thats purely personal prefference. Some people go naphtha first, then finish with couple of xylene/toluene pulls if they want jungle, some people go jungle and then re-x the amount they want of pure freebase, some people dont use tolu/xyle at all. I like working with limonene and salting out with FASI or FASW like BLAB tek.

You can combine all pulls in one, the disadvantage is that maybe later pulls are more impure, so you will 'average out' all the impurities (maybe your first pulls would come out white, but later more yellow, so if you just mix, maybe it all comes yellow. Not a problem though, you can always recrystallize). Another reason for not mixing everything is that for science's sake you might want to see how many mg each individual pull yields. Or another reason is that later pulls might be less saturated with DMT, so if you did many pulls and mixed them, maybe the amount of naphtha to dmt will be too large, and therefore not all DMT will precpitate. In that case, just pre-evap to, say, half the volume or whatever (depend on size of pulls. Also check FAQ), then freeze.

Good luck. And again: Dont throw anything away, thats the biggest mistake you can make. DMT can always be recovered

 

[whitebread420]

yes i understand what you mean about the DMT still being in the water, it's just so many impurities were visible and my know how was so little i just got rid of it...

so i wanna repeat the entire extract, and want to write a condensed tek and maybe have someone critique it for me?

per 500 g MHRB powder, boil it in 1 gallon pH 4 water (acidified with citric acid) for about five - eight hours. then allow some volume to evaporate. in my glass jug, i'll add 250 ml's of 20 M NaOH to make the overall solution pH 14, then add the MHRB solution. while the solution is still very hot, i will do 4 pulls with toluene and collect each pull into one Erlenmeyer flask.

this is the part where i want to implement the lex tek, because every time i'm always left with what is my guess to be all kinds of lipids and whatnot from the plant cells. with my toluene pulls i want to wash that with pH 4 water and collect the aqueous layers with a sep funnel to leave behind plant fats and oils. ill do this wash a few times. from here i'll add NaOH to the water i collected until the pH is 14 again. then once again i'll wash with toluene four times and collect each pull in a mason jar. from here the jars will be put into the freezer, and hopefully crystals will form.

i can then collect these crystals, put them in a test tube and recrystallize with minimal hot toluene. once again i'll put the hot toluene in a mason jar and stick that in the freezer for 48 or so hours.

so then hopefully ill be left with really pure crystals.

does this sound good?

 

[endlessness]

Nope, toluene doesn't freeze precipitate (and its neither good for recrystallizing) because dmt is too soluble in it even at freeze temperatures, and also it will dissolve impurities too well. So if you use toluene/xylene, then salt it out with FASA or vinegar, then convert that to the freebase. Or evaporate it instead of salting (nasty imo)

Freeze precipitation is done with heptane/hexane. Same with re-x. As linked above, 30ml warm solvent per g impure product.

 

[whitebread420]

ok. good to know.

so it's alright to start out with toluene, that is, use it for the initial extraction from the root bark mixture. but after the water wash from that it would be more wise to use heptane for the separation?

would ace brand VM&P naptha be a suitable substitute for heptane? (in either the secondary extraction from the water and for recrystallization?)

thanks a lot endlessness for your input so far.

 

[endlessness]

yeah you can use toluene first, then when you have your freebase jungle, use heptane to re-x the jungle till you get white crystals.

Im not from USA, and im not sure how much a brand such as ace vm&p naphtha can change their components (naphtha is a mix of aliphatic hydrocarbons, usually like pentane/hexane/heptane/octane and isomers). Some naphtha in some countries and brands may contain certain amounts of aromatics like xylene, which can screw up freeze precipitation, but from the years in this forum I think i've only read good things about ace vm&p naphtha.

I dont understand what you mean "secondary extraction from the water".. You mean after pulling with toluene from the main mimosa mix, doing more pulls with naphtha? No thats not good idea because toluene/xylene will already have picked up most of your alkaloid. You use the naphtha to pick up the stuff from your evapped (or salted and converted) toluene/xylene

 

[whitebread420]

ya you don't know what i meant, sorry.

i'm talking about after i wash the extract obtained with toluene with acidic water, i want to then separate the alks from the water with heptane/naptha, correct? then freeze it? then recrystallize.

 

[endlessness]

with acidic water you mean? because basic water will not wash the alkaloids away, just lye and polar impurities. If you mean with acidic water, then please call it "salting", its the standard word we use. Washing means the water (or whatever solvent used) will carry away impurities, while alkaloids remain undissolved.

So if you salt, then you have to either evaporate/dry the salt (like if its FASW or FASA or vinegar). If its FASW or FASA, you'll have solid fumarate crystals (or wax), if its vinegar/acetic acid, you might more likely have a goo. You can either keep (specially if its fumarates) for storage/oral taking (and if you want, wash the crystals with pure dry cold acetone or IPA), or you can convert the salt to freebase, as explained in BLAB tek in the wiki.

Once you convert to freebase, if you have an impure product, then yes you can use naphtha/heptane to recrystallize it. This will leave behind impurities and possibly some NMT/2-MTHBC (which can be active, so dont throw anything away). Naphtha/heptane will not dissolve dmt in salt form.

 

[whitebread420]

lol sorry you must have started your reply right before i edited my post ... yea i meant acidic water.