反应详情

温度

70 °C

1 g of sodium 3-acetoxymethyl-7-[2-(2-formylaminothiazol-4-yl)-2-methoxyiminoacetamido]-3-cephem-4-carboxylate were dissolved in 12 ml of 50% v/v aqueous methanol, and 20 g of calcium chloride dihydrate were added. The mixture was then stirred at 70° C. for 35 minutes, after which it was diluted with 30 ml of ice-water and insolubles were filtered off. The filtrate was acidified with hydrochloric acid and extracted three times, each time with 50 ml of ethyl acetate. The extracts were combined, washed with an aqueous solution of sodium chloride, dehydrated over anhydrous magnesium sulphate and concentrated by evaporation under reduced pressure. The residue was dissolved in ethyl acetate, and diethyl ether was added thereto. The resulting solid was separated, giving 0.6 g (yield 66.7%) of the title compound.

1. additionwere added
2. filtrationwere filtered off
3. extractionextracted three times
4. washwashed with an aqueous solution of sodium chloride
5. concentrationconcentrated by evaporation under reduced pressure
6. dissolutionThe residue was dissolved in ethyl acetate
7. additiondiethyl ether was added
8. customThe resulting solid was separated