Method of preparing delta-9-tetrahydrocannabinol esters
A technology of pyridine and compound, which is applied in the field of preparation of δ-9-tetrahydrocannabinol ester, can solve the problems of lack of efficacy and high price of soft gelatin capsule preparations, etc.
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Embodiment 1
[0012] To 1 gram of pure THC (about 95% pure) was added 1 g of succinic anhydride and 30 ml of pyridine and the reaction mixture was refluxed for 24 hours. The reaction mixture was poured into 100ml of ice water and extracted with diethyl ether (30ml×3), the diethyl ether extracts were combined, dried with anhydrous sodium sulfate and evaporated to dryness [TLC test using silica gel plates, developing solvent: hexane-diethyl ether (80 : 20), developer: fast blue solution, showing that its conversion rate is 30-40%]. The residue was mixed with 5 g of silica gel and 5 ml of ether, and the dried slurry was transferred to the top of a silica gel column (40 g of silica gel, size: 3×50 cm), and eluted with a mixture of hexane-ether in increasing polarity, mixed with hexane Alkane-diethyl ether (9:1) and diethyl ether were eluted and evaporated to give 0.442 g THC-HS (yield 33%).
Embodiment 2
[0014] To 1 g of THC (purity 95%) were added 0.5 g of anhydrous sodium carbonate, 1 g of succinic anhydride and 20 ml of dry benzene and the reaction mixture was refluxed for 24 hours. The reaction mixture was filtered and the filtrate was evaporated to dryness. Analysis by HPLC (C18 column, used methanol:water:acetic acid=80:20:0.01) showed that the THC-HS content of the residue was 17-20%.
Embodiment 3
[0016] To 1 g of THC (purity 95%) were added 0.5 g of succinic anhydride, 0.35 g of 4-pyrrolidinyl pyridine and 20 ml of benzene and the reaction mixture was kept at room temperature for 3 hours. TLC screen (Screening) showed that the content of THC-HS formed was about 20-30%, and the reaction mixture was allowed to stand overnight for about 24 hours before doing TLC test (the content of THC-HS was about 30-50%). Then the reaction mixture was refluxed for 4 hours (the content of THC-HS was 75.6%, HPLC analysis), after adding 0.30g 4-pyrrolidine pyridine, the reaction mixture was refluxed for 20 hours again, and the HPLC analysis showed that the content of THC-HS did not increase (about 75%).
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