Cycloastragenol new crystal form A and preparation method thereof
A technology of cycloastragalus and crystal form, which is applied in the field of organic chemical drug preparation, can solve the problems of non-compliance with green environmental protection, injury to operators, and many reaction steps, etc.
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Embodiment 1
[0039] Add 20.0g of cycloastragenol to 120mL of methanol solution, heat to 60°C-65°C until cycloastragenol is completely dissolved, add 500mL of petroleum ether and stir, slowly lower to 40°C-45°C and keep stirring for 30 minutes, then keep it for 8 hours ; Lower the temperature to 30°C to 35°C and continue to heat and stir for 40 minutes, then keep the heat to stand for 10 hours; drop to 20°C to 25°C and continue to heat and stir for 30 minutes, then keep the heat to stand for 10 hours; lower to 5°C to 10°C and continue to heat and stir for 30 Minutes, heat preservation and standing for 8 hours; finally lower the temperature to -8°C and continue heat preservation and stirring for 6 hours, filter, and vacuum dry at 40°C to obtain cycloastragenol crystal form A with a yield of 82.9% and a purity of 99.96%.
Embodiment 2
[0041] Add 20.0g cycloastragenol into 100mL ethyl acetate solution, heat to 60°C-65°C until cycloastragenol is completely dissolved, add 600mL water and stir, slowly cool down to 40°C-45°C and keep stirring for 30 minutes, then keep it for 10 minutes Hours; drop to 30°C-35°C and continue to keep warm and stir for 40 minutes, keep warm for 10 hours; drop to 20°C-25°C and continue to keep warm and stir for 30 minutes, keep warm for 10 hours; drop to 5°C-10°C and continue to keep warm and stir After 30 minutes, keep it warm for 8 hours; finally lower the temperature to 0°C, continue to keep warm and stir for 6 hours, filter, and dry under vacuum at 40°C to obtain cycloastragenol crystal form A with a yield of 81.8% and a purity of 99.92%.
Embodiment 3
[0043]Add 20.0g of cycloastragenol to 800mL ethanol solution, heat to 60°C-65°C until cycloastragenol is completely dissolved, add 1000mL of n-hexane, stir and slowly cool down to 40°C-45°C, keep stirring for 30 minutes, keep the temperature for 6 hours; Lower the temperature to 30°C to 35°C and continue to heat and stir for 40 minutes, and then keep it for 10 hours; lower it to 20°C to 25°C and continue to heat and stir for 30 minutes, and keep it for 10 hours; lower it to 5°C to 10°C and continue to heat and stir for 30 minutes , heat preservation and standing for 10 hours; finally lower the temperature to -10°C, continue heat preservation and stirring for 6 hours, filter, and vacuum dry at 40°C to obtain cycloastragenol crystal form A with a yield of 80.4% and a purity of 99.94%.
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