Synthesis method of cefepime hydrochloride
A technology for the synthesis of cefepime hydrochloride and its synthesis method, which is applied in the field of synthesis of cefepime hydrochloride, can solve the problems of increased impurities and decreased content, and achieve the effects of increased purity, improved quality, and improved yield
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Embodiment 1
[0027] At room temperature, mix 500ml of water, 600ml of dimethylformamide and 1200ml of isopropanol evenly, add 150g of 7-MPCA and 200g of AE-active ester under effective stirring to form a fluid slurry system; drop 20% Sodium hydroxide until the pH of the solution system is between 5.5 and 6.5, react at 20°C for 4h; continuously extract three times with 3000ml of dichloromethane, and distill the water phase under reduced pressure at room temperature at 20°C to 25°C for 1.5h; then add 6mol / L of Adjust the pH value to 0.5-1.0 with hydrochloric acid, then add 2.5 L of acetone, stir for 2 hours, crystallize to obtain cefepime hydrochloride, filter with suction, wash the filter cake with acetone, and then dry it for 1 hour to obtain 210 g of cefepime hydrochloride. 99.5%.
Embodiment 2
[0029] Put 140g of 7-MPCA and 180g of AE-active ester in a mixed solvent of 1500ml of dimethylacetamide and 500ml of water, stir and homogenize; adjust the pH to 6.0-7.5 with triethylamine, and react at 15°C for 3h; add 2500ml Dichloromethane was extracted twice, and the water phase was distilled under reduced pressure at 10-20°C for 1.2h; then, 6mol / L hydrochloric acid was added to control the pH value to 1.0-1.6, and 2.6L acetone was added, stirred for 2.5h, and crystallized to obtain hydrochloric acid Cefepime was filtered with suction, and the filter cake was washed with acetone and then dried for 1 h to obtain 295 g of cefepime hydrochloride, with a purity of 99.7% by HPLC.
Embodiment 3
[0031] Mix 400ml of water, 480ml of dimethyl sulfoxide and 800ml of methanol evenly, add 120g of 7-MPCA and 160g of AE-active ester; under effective stirring, add aqueous sodium bicarbonate solution dropwise, and adjust the pH value of the reaction solution to between 6.0 and 7.0 , acylation reaction at 30°C for 6h; then add 2000ml of dichloromethane for extraction twice, combine the water phases and distill under reduced pressure for 2h at 0-5°C; after the reduced-pressure distillation, add 6mol / L hydrochloric acid to adjust the pH to 0.6 to 1.5, add 2.2L of acetone and stir for 1.5 hours, crystallize to obtain cefepime hydrochloride, filter and dry with suction for 1 hour to obtain 170 g of cefepime hydrochloride, the purity of which is 99.6% by HPLC.
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