反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
The solution of benzhydryl 7-[2-(6-aminopyridin-2-yl)-2-tert-butoxycarbonylmethoxyiminoacetamido]-3-ethylthio-3-cephem-4-carboxylate (syn isomer, 2.3 g) in trifluoroacetic acid (10 ml) and anisole (2 ml) was stirred for 2 hours at ambient temperature. The resultant solution was poured into diisopropyl ether (300 ml) and the precipitates were collected by filtration. The precipitates were dissolved in an aqueous solution of sodium bicarbonate (pH 7.5). The aqueous solution was washed with ethyl acetate and was adjusted to pH 2.3 with 10% hydrochloric acid. The precipitates were collected by filtration, washed with water and dried over phosphorus pentoxide under reduced pressure to give 7-[2-(6-aminopyridin-2-yl)-2-carboxymethoxyiminoacetamido]-3-ethylthio-3-cephem-4-carboxylic acid (syn isomer, 0.87 g), mp. 164° to 167° C. (dec.).
WORKUP
后处理
- filtrationthe precipitates were collected by filtration
- dissolutionThe precipitates were dissolved in an aqueous solution of sodium bicarbonate (pH 7.5)
- washThe aqueous solution was washed with ethyl acetate
- filtrationThe precipitates were collected by filtration
- washwashed with water
- dry with materialdried over phosphorus pentoxide under reduced pressure