Okay I have two questions regarding the fisher indole rxn for DMT vs 5-meo-DMT. One question regarding the masked aldehydes protected as the diethyl acetal derivatives and another question regarding the a organic solvent used to extract the free base from the acidic aq. soln.
Question 1: are the protected aldehydes used in both indole rnxs the same (DMT vs 5-meo-dmt)?
1. 5-MEO-DMT (this info was taken from a thread created by
@William Dampier(http://bbzzzsvqcrqtki6umym6itiixfhn...synthesis-of-5‐meo-dmt-via-fischer-indole.11/)
In this rxn, they use 4,4-diethoxy-N,N-dimethyl-butan-1-amine (CAS Number: 1116-77-4 ) and 4-methoxyphenylhydrazine hydrochloride
2. DMT (this info as taken from a thread created by
@halohydrin (xmrhfasfg5suueegrnc4gsgyi2tyclcy5oz7f5drnrodmdtob6t2ioyd.onion/)
In this rxn, they use (N,N-dimethylamino)butanal diethyl acetal (CAS Number: 1116-77-4)
Now... it seems as thought the only differences in these two fisher indoles (DMT vs 5-MEO-DMT) are the types of phenylhydrazines used. So then, im assuming CAS Number: 1116-77-4 can be used for both? I guess I just answered my own question, but just need confirmation. I accidentally ordered a close cousin of CAS Number: 1116-77-4,
4-(N,N-Dimethylamino)butanal Dimethyl Acetal (CAS 19718-92-4).
Question 2: Solvents used for tryptamine extractions
From
the 5-meo-dmt procedure ,
"13. The suspension was extracted with
2-MeTHF (3x1.45 L, 10.0 vol); following each extraction, the layers were allowed to settle for 15 min, the lower alkaline water layer was separated into a drum, and the upper organic layer was collected.
14. The lower aqueous layer was discarded and the combined
2-MeTHF organic layers were transferred to a 20 L-flask.
15. The solution was concentrated in vacuo to an oily amber residue.
16. Residual water was removed azeotropically by redissolving the residue with fresh
2-MeTHF (1.45 L, 10 vol) and repeating the concentration step.
17. This oily residue was dried on the rotatory evaporator under vacuum (10−20 mbar) for 1 h at 40−45 *C to provide 117.68 g (64.9% theoretical yield) of crude 5-MeO-DMT freebase."
From the DMT procedure:
"9. suspension is extracted with 3*1.45 L 2-Me-THF,
which can be substituted by isopropyl acetate or DCM.
10, The organic layers ar combined and solvented is striped off by distillation. The remaining oily residue is redissolved in solvent and reconcentrated (to remove water azeotrope)."
Can this same substitution be applied to extracting the 5-meo-dmt freebase and are there solvents that can be used (I know certain solvents can actual form unwanted intermediates).
-I do not want to use 2-me-thf since its pricey (although I did use it for the 5-meo-dmt freebase extraction procedure but ended up with a thick oil, which when vaporized, it was for sure 5-meo-dmt
-I tried using isopropyl acetate for the DMT free base, but for the love of god it takes AGES to evaporate!! I left it in the vacuum oven at 30-40 mbarr for 24 hours and 75% of it evaporated. I even put it in the roto vap at 1MPa at 40C for 3 hours...it did evaporate a little. Then I said fuck it and cranked the water bath to 86C and it still would not evaporate!!
Some solutions:
extract the DMT freebase in the isopropyl acetate solution (assuming i didnt vaporize the rest of the DMT freebase lol) DCM from the isoporpyl acetate solution) with DCM. I would have to compare the partition coefficients with the two solvents with respect to DMT
Start over and use DCM for the extraction.