SWIM has been iso alcohol extracting MHRB with a soxhlet and then doing A/B with muric acid / sodium carbonate. SWIM then extracts the basified mixture with DCM in a heavyer than water liquid / liquid extractor. Swim does not wish to go though the ong evap process, but rather migrate the dmt to another solvent that would be capable of freeze precipitation. Is this possible?

if this were possible, the dmt wouldn't freeze precipitate in the solvent because it would be more soluble in it than in dcm. the principle of freeze-precipitation is to get a solute to "crash out" (aggregate as crystals in solution), because it's not very soluble in the solvent.

Would it be possible to Add naptha to the dcm, Distill off the DCM and then freeze precip the naptha?

if thats what you want to do, it may be easier to distill off the DCM first then dissolve solids in naptha for freeze precipitation.

^^ exactly.

let the dcm evaporate, redissolve the residue in hot naptha, then collect and freeze precipitate

The residue really seems to be sticking to the inside of the flask.. im heating the naptha right now but it sure is stuck on there..

what color is your saturated DCM typically? using the liquid/liquid extractor got mine all the way to brown..

iunno, never used DCM. maybe try and redissolve what didnt in the naptha into more DCM and evap in a dish.

Oh.. great. I'm getting advise on what to do from someone who's never done it. Thanks. Looks like this batch is screwed.

Does anyone else who knows from USING DCM, how to migrate it out other than evapping? Distilling off at 104 clearly results in an undissolveable tar.

many apologies. i should have said upfront that I dont extract with DCM. though it should make sense that if there was DMT in the DCM, once evaporated there should be some in the solids which would then redissolve in naptha.

i dont know the solubility of the natural salts of DMT, im assuming DMT tannate, in isopropyl as you did as an initial extraction step. Did you freebase the bark before soxhleting in ISO? is DMT soluble in ISO in its natural form found in MHRB?

I assume that's fahrenheit

so now you're aware, dcm pulls other alkaloids as well as dmt. now you should dissolve the 'tar' in a small amount of hot bestine, and put it in the freezer. if your extraction went well, you'll find some very active off-white crystals by the next day.

worked for swim.

does dcm pull anthing that is active that either tolulene and xylene dont ?
what is the diff between what is pulled with xylene and tolulene ?

heres a list of xlogp's that i grabbed from one of 69ron's posts in: http://www.dmt-nexus.me/...261&f=14&q=46544


here are xlogp of solvents and more alks from ron69: (check post 3)
http://www.dmt-nexus.me/....aspx?g=posts&t=1574

id guess that DCM pulls DMT freebase more readily b/c of its lower xlogp, this should work the same with more "jungle spice" being pulled also. More junk and additional mystery alks (the lists above are good but still limited, who knows fully whats in MHRB) may be pulled as well due to the lower xlogp possibly accounting for the brownness in your DCM pull.

a SWIM once told a friend of mine that xylene has yielded brownness of tan to caramel to coffee colored before that is quite active.

dcm is slightly more polar than both toluene and xylene (which don't differ very much). dcm is used to extract a wide variety of alkaloids, from mescaline to caffeine. it's a very versatile solvent.

to purify compounds, recrystallization is done.. or column chromatography then recrystallization.
column chromatography requires a binary solvent mixture, something like ethyl-acetate and methanol. for all practical purposes, using bestine to clean it up is tried and true; there are several threads on this

Hmm... so according to this list of solvent XLogP3 data, using a CLLE di-ethyl ether will make mostly n,n-DMT products and DMT-n,Oxide. With DCM and chloroform being more able to extract along with the n-oxide and n,n the jungle spice and more "mystery alks?" Sorry, does it show that I am confused?

no, you're right

dmt will be more soluble in both dcm and chloroform than in ether...unfortunately, so will the other alkaloids

I wonder how many times SWIY defatted before using DCM on the basified solution.

Also, I'd like to know what people think about defatting (don't feel the need to make a whole new thread). If SWIM were to defat with DCM on an acidic h2o solution (including a small remnant of IPA from a soxhlet extraction) using a FBF and hotplate stirrer, how many pulls, what volume of NP, at what temperatures, etc.? After this mixing, the two layers would be separated in a separatory funnel.

never use dcm to defat
you will likely hurt your yields. save the dcm for extracting the free base.

instead use something with a higher xlogp like naptha for defatting. it's perfectly fine to use different solvents for different tasks.

swim doesn't do a defat with MHRB, not many people do. but when they do, its typically with naptha or xylene.

Hai guys, this is SWIM's first post. He's just an amateur kitchen kemist that has been lurking these forums for quite a while now. Let SWIM point out upfront that he does not have any experience with DCM.

From what SWIM's been reading, it should be very possible to use DCM in the extraction stage using the CLLE (after proper defatting), after which one would distill the DCM until a small concentrated DMT-rich amount is left over, due to DCM's BP being lower than that of DMT.

Once SWIY reaches that stage, one would add another solvent, like cold acetone (or maybe Heptane). until the freshly added solvent starts to distill, one would let it evaporate.

SWIM's guess is, if left over with a lot of gunk, either the defatting didnt go optimal, or the destillation process was run for too long. e.g. dry-cooking (note the use of 'guess' xD)

SWIM thinks it was ron69 that pointed these techniques out, and has the most experience with this kind of thing, so maybe ask him for more detailed info.