HRID1902924

反应详情

EQUATION

反应方程式

HRID 1902924 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

420 mg (1.21 mmoles) of 3-methyl-7-phenylacetamido-3-cephem-4-carboxylic acid-1-oxide were silylated by stirring at 30° C. for 1.5 hours in 60 ml of 1,2-dichloroethane with 1.0 g (4.3 mmoles) of N-trimethylsilyltrichloroacetamide. The slightly yellow, substantially clear solution obtained was cooled in an ice-bath and bromination was carried out in 15 minutes using 250 mg (0.87 mmole) of 1,3-dibromo-5,5-dimethylhydantoin as the brominating agent. During the bromination reaction, the mixture was irradiated with a 520 W fluorescent lamp to obtain a 48% yield of trimethylsilyl 3-bromomethyl-7-phenylacetamido-3-cephem-4-carboxylate-1-oxide.

WORKUP

后处理

  1. customThe slightly yellow, substantially clear solution obtained
  2. temperaturewas cooled in an ice-bath
  3. customDuring the bromination reaction
  4. customthe mixture was irradiated with a 520 W fluorescent lamp