HRID255474

反应详情

EQUATION

反应方程式

HRID 255474 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
40 °C

PROCEDURE

实验过程

To a suspension of 200 mg (0.35 mmole) of 7β-[2-(2-aminothiazol-4-yl)-2-(4-chlorobenzyloxyimino)acetamido]-3-acetoxymethyl-3-cephem-4-carboxylic acid in 5 ml of methylene chloride was added 0.5 ml of MSTFA and the suspension was stirred at 40° C. until solution occurred. The solution was cooled to room temperature and 0.13 ml (0.87 mmole) of TMSI was added. The reaction stirred at room temperature for 30 minutes and evaporated to an oil. The oil was dissolved in 3 ml of acetonitrile and 0.12 ml (1.5 mmole) of THF was added. The mixture was then stirred at room temperature for 5 minutes to destroy excess TMSI and provide in solution the corresponding 3-iodomethyl-3-cephem derivative.

WORKUP

后处理

  1. temperatureThe solution was cooled to room temperature
  2. stirringThe reaction stirred at room temperature for 30 minutes
  3. customevaporated to an oil
  4. dissolutionThe oil was dissolved in 3 ml of acetonitrile
  5. stirringThe mixture was then stirred at room temperature for 5 minutes
  6. customto destroy excess TMSI