Fresh cacti, w/ a water content of 90-95%, are difficult to handle; the juice is not easily separated from the fibers, and the presence of mucilaginous substances causes trouble during extraction. Thus, it is preferable to dry the plants immediately after they are collected, in order to avoid losses and deterioration. The plants should be cleaned, the spines extracted with nippers, and the remaining material cut in thin slices and dried in the sun or better in a low-temperature drier (40-60oC). The dried substance is easy to grind, and the powder can be stored if neccessary.
The powdered material (10kg) was exhaustively extracted in a percolator with hot, acidulated [0.3% acetic acid] 96% ethanol, the extract filtered and concentrated in vacuo to 500 mL. water was added (2.5L) and concentrated again to 2.3L. The solution was filtered to separate oils, resins, chlorophyll, etc and washed twice w/500mL of chloroform. The aqueous solution was neutralized with solid potassium carbonate, and an excess of 20g was added. A precipitate containing only calcium carbonate was eliminated, and the solution extracted four times with the same volume of cholorform (2.3L). The combined [chloroform] extracts, after having been dried [allowed to stand over] with anhydrous sodium sulfate were concentrated to 780mL and filtered. The solution was extracted twice with 150 mL of 3% aqueous HCl and once with 100 mL water. The aqueous solution was washed with ether repeatedly and filtered. This is the purified aqueous solution of total alkaloids. [This would be a good place to slowly evaporate the water and consume the residue, for further purification of the alkaoids, see below...By the time all the water is removed, there should be no excess HCl around.]
This soln. is alkalinized agin with dry potassium carbonate an extracted 5 times with 500 mL of ether. This extract, containing the ether soluable alkaloids, was concentrated to 500 mL. this is A (trichocereine) [this is mostly the more lipid soluable, inactive, dimethyl-mescaline, aka trichocercine]
The aqueous solution [still basic] is extracted three times with 500 mL chloroform, and the extract concentrated to 200 mL; this is soln B (mescaline) [this could be taken to dryness to give mescaline base, probably mostly pure]
Soln B was extracted twice with 40 mL of 5% aq. HCl and once with 20 mL water. The aqueous extract was then washed with 20 mL chloroform and 20 mL ether. After alkalinization with potassium carbonate, the solution was extracted with chloroform and the [chloroform] extract evaporated to dryness. It weighed 4g. After neutralization with alcholic hydrochloric acid, the crude hydrochloide was dissolved in 30 mL. of absolute [ethyl] alcohol and the filtered solution overlayed with 30 mL of ether. The hydrchloride crystallized. re-xtalized from alcohol, the pure salt melted and 181-182oC.
L. Reti Journal of the American Chemical Society, 1951, p 1767
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