Crystallization purification method for paclitaxel
A purification method, paclitaxel technology, applied in the field of compound crystallization, can solve the problems of high equipment requirements, no purification effect, poor purification effect, etc.
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Embodiment 1
[0060] Weigh 10g of paclitaxel (HPLC purity 93%, 7-epitaxol is 0.12%), add 44ml of dichloromethane, 88ml of acetone, heat to 40°C to dissolve, cool to 25°C, add dropwise 264ml of n-hexane to make it crystallize, After the dropwise addition was completed, the temperature was lowered to 5° C., filtered, and vacuum-dried at 50° C. to obtain 9.20 g of a white solid with an HPLC purity of 97.5% and 0.091% of 7-epitaxel. The molar yield is 92%.
Embodiment 2
[0062] Weigh 5g of paclitaxel (sample in Example 1), add 22ml of dichloromethane and 44ml of acetone, heat to 40°C to dissolve, cool to 25°C, add dropwise 110ml of n-heptane to crystallize, dropwise complete, cool to 5 °C, filtered, and vacuum-dried at 50 °C to obtain 4.66 g of a white solid with an HPLC purity of 99.5% and 0.088% of 7-epitaxel. The molar yield is 93.2%.
Embodiment 3
[0064] Weigh 10g of paclitaxel (HPLC purity 93%, 7-epitaxol is 0.12%), add 44ml of chloroform, 88ml of acetone, heat to 40°C to dissolve, cool to 25°C, add dropwise 264ml of n-hexane to crystallize, add dropwise After completion, the temperature was lowered to 5° C., filtered, and vacuum-dried at 50° C. to obtain 9.20 g of a white solid with an HPLC purity of 97.1% and 0.105% of 7-epitaxel. The molar yield is 92.2%.
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