HRID1278321

反应详情

EQUATION

反应方程式

HRID 1278321 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 12.8 g. (31.5 mmole) of p-nitrobenzyl 7-amino-3-chloro-3-cephem-4-carboxylate hydrochloride in 115 ml. of dry DMF were added with stirring 10.4 g (6.5 ml., 72 mmole) of phosphorus trichloride. The reaction mixture was stirred at room temperature for about 2 days and was then dispersed in a mixture of 5% aqueous sodium bicarbonate and ethyl acetate. The organic layer was separated and treated with 1 N hydrochloric acid. The title compound precipitated from solution and was filtered and dried under vacuum. There were obtained 11.3 g. (67% yield) of the salt.

WORKUP

后处理

  1. customThe organic layer was separated
  2. additiontreated with 1 N hydrochloric acid
  3. customThe title compound precipitated from solution
  4. filtrationwas filtered
  5. customdried under vacuum
  6. customThere were obtained 11.3 g