HRID1902912

反应详情

EQUATION

反应方程式

HRID 1902912 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

255 mg of N-trimethylsilylcaprolactam (1.36 mmoles) were added to a refluxing suspension of 360 mg (1.03 mmoles) of 3-methyl-7-phenylacetamido-3-cephem-4-carboxylic acid-1-oxide in 25 ml of dichloromethane and a clear, colorless solution was obtained within 2 minutes. Refluxing was continued for another 25 minutes and the solution was cooled in an ice-bath and diluted to 40 ml with dichloromethane 150 mg of amidosulfonic acid (1.53 mmoles) were added thereto and bromination was carried out in half an hour using 299 mg (1.68 mmoles) of N-bromosuccinimide as the brominating agent to obtain a 51% yield of trimethylsilyl 3-bromomethyl-7-phenylacetamido-3-cephem-4-carboxylate-1-oxide.

WORKUP

后处理

  1. customa clear, colorless solution was obtained within 2 minutes
  2. temperatureRefluxing
  3. temperaturethe solution was cooled in an ice-bath
  4. additionwere added
  5. waitbromination was carried out in half an hour