Butyl acetate works for the pulls from the cactus/ lime paste. There's a possible drawback with citric acid's rather lower solubility in the BA, but one workaround is:
Thank you very much, there is a chance i get Ethyl Acetate next week, but if I don´t succeed i´ll try the Butyl, thanks, im very new to this processes, i hope everything works good!Butyl acetate works for the pulls from the cactus/ lime paste. There's a possible drawback with citric acid's rather lower solubility in the BA, but one workaround is:
This is all somewhat experimental, so some nuances may have been overlooked in the description. Also, everything will stink of bananas
- to deliberately wet more BA by shaking it with ~2% of distilled water by volume,
- decanting away from excess water,
- saturating the 'wet' BA by either shaking it with excess citric, or percolating it through a small column filled with citric
- adding this"CASBA" solution to the pulls of cactus extract liquid should lead to precipitation of mesc citrate but
- if the pulls are too dry, citric acid may co-precipitate(?)
Getting EA would be ideal, but I'd equally be delighted if other researchers were to experiment with using BA.
Butyl acetate works for the pulls from the cactus/ lime paste. There's a possible drawback with citric acid's rather lower solubility in the BA, but one workaround is:
This is all somewhat experimental, so some nuances may have been overlooked in the description. Also, everything will stink of bananas
- to deliberately wet more BA by shaking it with ~2% of distilled water by volume,
- decanting away from excess water,
- saturating the 'wet' BA by either shaking it with excess citric, or percolating it through a small column filled with citric
- adding this"CASBA" solution to the pulls of cactus extract liquid should lead to precipitation of mesc citrate but
- if the pulls are too dry, citric acid may co-precipitate(?)
Yes this works with acetone, at least for precipitating harmala citrate and should work similarly for mescaline too. It should also be pretty easy to separate the acetone from the BA if you have a small fractionation column, and maybe even just with simple distillation, since there's a healthy 70°C separation between their respective boiling points.
Yes, that's the right way to wet the BA. I've separated it from any remaining droplets of water before moving on to the next step, but even this might not be necessary.
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Might well do, since it won't be much of an amount of acetone to provide the requisite amout of CA anyhow. Small losses of BA co-solubility in water will probably (definitely) occur.
Thank you very much, this is very helpful, I´ll try to record my process. On the other hand I found out is suposetly pretty easy to make some ethyl acetate by mixing acetic acid and ethanol. The known synthesis uses sulfuric acid as a cathalyzer, but for what I know now the reaction will happen without it, it would just take more time. Just did that, I will know for sure in a few days.Yes this works with acetone, at least for precipitating harmala citrate and should work similarly for mescaline too. It should also be pretty easy to separate the acetone from the BA if you have a small fractionation column, and maybe even just with simple distillation, since there's a healthy 70°C separation between their respective boiling points.
Yes, that's the right way to wet the BA. I've separated it from any remaining droplets of water before moving on to the next step, but even this might not be necessary.
I made the CASBA both by running the wet BA through a tube loosely packed with CA, held in place at the bottom with a plug of cotton wool, or more simply by dumping a slight excess of CA into a flask of wet BA. If all the CA dissolves, you can always add a dash more until a few crystals refuse to dissolve. I don't know if the CA increases the solubility of water in BA, but it might do. Much commercial citric acid is the monohydrate, which may have a small effect on the overall balance of things. Using anhydrous citric acid would remove some of the water from the BA, potentially reducing its solubility.
So, now you have some CASBA you may want to work out how much CA you've dissolved in each unit volume. These kinds of figures tend to prove useful in the long run, so they're worth recording (except I didn't
You can add your CASBA to the cactus pulls in aliquots at first and then dropwise until no additional clouding is observed.
I think there's a higher risk of excess CA co-precipitating with the mesc citrate when using BA, because the citrate takes water out of the solution as water of crystallisation while it crystallises. It may be worthwhile wetting at least one portion of the cactus extract to see if it performs any better, or any worse of course.
This is an experimental method, which means you'll be experimenting too. Should you decide to try out these suggestions, it'll be very helpful if you record all that you attempt in maximum detail, including 'failures'. And remember - don't throw anything away until you're absolutely sure you've got the goods. Recycle your solvents too - it'll be broadly similar to the EA clean up describe either in the CIELO thread itself or from a link buried somewhere in that mountain of a thread.
The main problem with Fischer esterification in making EA is that it's an equilibrium process and the removal of unreacted ethanol from the EA is highly challenging, since they have very similar boiling points.
Thanks for that last tip. Would there still be any problem with using ethyl acetate with some residual ethanol in the CIELO process? If so, I'll be sure to use more acetic acid to ensure the ethanol is converted.
Yes, I think EA with too much free ethanol would cause poor yields and separation problems due to its miscibility with water. 'Too much' is probably a low single figure percentage, at that.
