An1cca said:
...The conclusion is that an ammonia-free route to THH synthesis IS possible by first precipitating the Zinc-ions as carbonate with sodium BIcarbonate, filtering them off and then precipitating the THH out of solution with sodium carbonate. That is, if THH is not precipitated by sodium carbonate (as is indeed suggested by the experiments of VDS)...
The underlined should be sodium BIcarbonate I presume. I had myself edited so often, these words mingle up so easily LOL.
Good thinking & tinkering by the way
VDS suggested that sodium BIcarbonate would not precipitate THH but would precipitate harmaline (this was his criticism on the "popular internetsites" ). The 'distance' between harmine-THH should be bigger than harmine-harmaline, this is indeed also reflected by
Nitegazer's TLC's.
So your efforts indicate there's a full ammonia free route if we first separate harmaline from harmine. Set harmine aside, reduce the harmaline. Precipitate the ZnOH or ZnCO3 and filter off. Then precipitate the THH. So actually 2 separation steps necessary. Yet separating harmine-harmaline in advance needs tact according to VDS paper.
Or..
Have the harmine+ZnOH (or harmine+ZnCO3) precipitated together and separate those later a la manske.
[**]
What I also would like to do is to see how a full precipitation of ZnOH or ZnCO3 (not dry but still in suspension) behaves when ammonia gets pored on. I did those experiments on a smaller scale (1 ml ammonia was enough) successfully but would like to do it in real-scale. If this works as well as a complete ammonia-only basing, it could reduce the use of the amount ammonia substantially.
[**] If this works great then a manske could be replaced with just adding some ammonia (amount to be established) to the harmine+ZnCO3 mixture and filter. Not ammonia free but close. Has to be checked.
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If people want to make use of the harmala "depressions" as a separation indicator, I would suggest a pH meter with 0.01 resolution. Forget pH strips to make any separation. And also not to work with too strong a base (as is my 8mol/L) because I've found to very easily overshoot a depression, making it myself more difficult.
The neat thing about those depressions is that the calibration at absolute values becomes less important and the shape-behavior of the curve chimes in as a give away. Yet one can not go around this ghetto style, some more
fingerspitzengefühl is welcome.
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To come to a "guide" or tek, I think we could make a distinct in 2 ways:
1) a route of strict minimal fuzz, the fast way, no separation steps, reducing harmine+DHH into harmaline+THH, base with ammonia only, filter & wash. It even allows for having no pH checking at all if one just uses enough dirt cheap ammonia, wash well afterwards. One just doesn't know the harmine/THH ratio but this is for when you don't care. I had a blast of a pharma session with it.
2) for those who want harmine and THH separately: including the several separation steps, likely better pH metering, more fingerspitzengefühl, more time consuming ...
