HRID1905800
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 0 °C
PROCEDURE
实验过程
To a suspension of 3-hydroxy-7beta-phenylacetylaminocepham-4-carboxylic acid diphenylmethyl ester (2) in dichloromethane (9 parts) cooling at 0° C. are added pyridine (6 equivalents) and toluenesulfonyl chloride (6 equivalents). The mixture is let stand at 0° to 5° C. for 105 hours. The reaction mixture is diluted with ice-water, the organic layer is taken, washed with hydrochloric acid and water, dried, and concentrated. The residue is crystallized from a mixture of ethyl acetate and hexane to give 3-p-toluenesulfonyloxy-7beta-phenylacetylaminocepham-4-carboxylic acid diphenylmethyl ester (3d). Yield: 84.7%. mp. 133°-136° C. (decomposition).
WORKUP
后处理
- washwashed with hydrochloric acid and water
- customdried
- concentrationconcentrated
- customThe residue is crystallized from a mixture of ethyl acetate and hexane