Aceclofenac preparation method
A technology of aceclofenac and acid hydrolysis, which is applied in the field of preparation and purification of aceclofenac, can solve the problems of high environmental protection pressure, low product yield, complicated operation, etc., achieve low equipment corrosion, reduce impurity content, highly controllable effect
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Embodiment 1
[0029] The preparation of embodiment 1 aceclofenac
[0030] Add 500g of tert-butyl aceclofenac to a 2L three-necked flask, under stirring, add 500ml of acetic acid, 15ml of concentrated hydrochloric acid solution (mass fraction is 36%), 500ml of acetic anhydride, heat up to 50°C for 4h, cool to 10°C Stir and crystallize at -30°C for 2h, filter with suction, rinse the filter cake with an appropriate amount of purified water, and dry it in vacuum at 50°C for 8h to obtain 419.2g of white solid, which is the crude product of aceclofenac, with a yield of 97.3% and a purity of 99.82% by HPLC. . The maximum single impurity is 0.03% of aceclofenac tert-butyl ester.
[0031] Add 419.2g of crude aceclofenac and 840ml of acetic acid into a 2L three-necked flask, heat until the solid dissolves, add 4.2g of activated carbon after dissolution, keep stirring for 1 hour, then suction filter while it is hot, cool the filtrate to 25°C, stir and crystallize for 4 hours, After suction filtratio...
Embodiment 2
[0032] The preparation of embodiment 2 aceclofenac
[0033] Add 500g of tert-butyl aceclofenac to a 2L three-necked flask, under stirring, add 500ml of acetic acid, 25ml of concentrated hydrochloric acid solution (mass fraction is 37%), 500ml of acetic anhydride, heat up to 60°C for 3h, cool to 10°C Stir and crystallize at -30°C for 2h, filter with suction, rinse the filter cake with an appropriate amount of purified water, and dry in vacuum at 50°C for 8h to obtain 418.3g of white solid, which is aceclofenac, with a yield of 97.1% and a purity of 99.80% by HPLC. The maximum single impurity is 0.04% of aceclofenac tert-butyl ester.
[0034] Add 418.3g of crude aceclofenac and 840ml of acetic acid to a 2L three-necked flask, heat until the solid dissolves, add 8.4g of activated carbon after dissolution, keep stirring for 1 hour, then suction filter while it is hot, cool the filtrate to 25°C, stir and crystallize for 4 hours, After suction filtration, the filter cake was rinsed...
Embodiment 3
[0035] The preparation of embodiment 3 aceclofenac
[0036] Add 500g of aceclofenac tert-butyl ester to a 5L three-necked flask, under stirring, add 1500ml of formic acid, 100ml of concentrated hydrochloric acid solution (mass fraction is 38%), 850ml of acetic anhydride, heat up to 50°C for 6h, cool to 10°C Stir and crystallize at -30°C for 2 hours, filter with suction, rinse the filter cake with an appropriate amount of purified water, and dry it in vacuum at 50°C for 8 hours to obtain 417.0 g of white solid, which is the crude product of aceclofenac. The yield is 96.8%, and the HPLC purity is 99.71%. . The maximum single impurity is 0.07% of aceclofenac tert-butyl ester.
[0037] Add 417.0g of crude aceclofenac and 840ml of formic acid to a 2L three-necked flask, heat until the solid dissolves, add 8.4g of activated carbon after dissolution, keep stirring for 1 hour, then suction filter while it is hot, cool the filtrate to 25°C, stir and crystallize for 4 hours, After suc...
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