A kind of improved preparation technology of cefmetazole intermediate
A technique for preparing cefmetazole and its preparation process, which is applied in the field of improved preparation process of cephalosporin compound intermediates, can solve the problems of large amount of silanization reagents, heavy environmental pollution, and high single-step cost, and achieve single-step cost reduction and pollution reduction , Yield and Purity Improvement
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Embodiment 1
[0036] Intermediate III (by feeding 25 g of intermediate I, intermediate III prepared by the method described in Test Example 1) was dissolved in 400 ml of ethyl acetate, and dry HCl gas was passed into the reaction liquid, and the temperature was slowly raised to 40 ° C, and kept React at 40°C until the reaction is complete (1.5~2h), stop the reaction, cool the reaction to -20°C, add 300ml of ice water, 100ml of ethyl acetate, stir at 8-10°C for 30min, separate layers, and extract the water layer with ethyl acetate When there is no product, combine the organic layers, wash with saturated brine, dry, filter with suction, wash the filter cake with ethyl acetate, and concentrate the filtrate to dryness at 5~10°C to obtain oily intermediate IV with a yield of 94% and a purity of 96 %.
Embodiment 2
[0038] Intermediate III (25 g of Intermediate I, prepared by the method described in Test Example 1) was dissolved in 400 ml of ethyl acetate, and 46 ml of dry 2N HCl ethyl acetate solution was passed into the reaction solution (phase Ratio to intermediate III molar equivalent is 2.0eq), slowly heat up to 40°C, keep at 40°C until the reaction is complete (1.5~2h), stop the reaction, cool the reaction to -20°C, add 300ml of ice water, 100ml of ethyl acetate , stirred at 8-10°C for 30 minutes, separated layers, extracted the aqueous layer with ethyl acetate until no product was found, combined the organic layers, washed with saturated brine, dried, and suction filtered, the filter cake was washed with ethyl acetate, and the filtrate was separated in 5~ Concentrate to dryness at 10°C to obtain oily intermediate IV with a yield of 95% and a purity of 95.5%.
Embodiment 3
[0040] Intermediate III (25 g of intermediate I, prepared by the method described in Test Example 1) was dissolved in 400 ml of ethyl acetate, and 207 ml of dry 2N HCl ethyl acetate solution was passed into the reaction solution (phase Ratio to intermediate III molar equivalent is 9.0eq), slowly heat up to 40°C, keep at 40°C until the reaction is complete (1.5~2h), stop the reaction, cool the reaction to -20°C, add 300ml of ice water, 100ml of ethyl acetate , stirred at 8-10°C for 30 minutes, separated layers, extracted the aqueous layer with ethyl acetate until no product was found, combined the organic layers, washed with saturated brine, dried, and suction filtered, the filter cake was washed with ethyl acetate, and the filtrate was separated in 5~ Concentrate to dryness at 10°C to obtain oily intermediate IV with a yield of 93.7% and a purity of 96.5%.
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