HRID648189

反应详情

EQUATION

反应方程式

HRID 648189 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 54.6 g (0.29 mole) ethoxy carbonyl methanesulfonyl chloride in 250 ml methylene chloride is stirred at 0° under a nitrogen atmosphere while 46.8 g (0.29 mole) hexamethyldisilazane is added dropwise. The resulting cloudy solution is allowed to warm to 25° over one hour and then evaporated in vacuo to an oil which crystallizes: yield of the title product is 48.4 g (100%), mp 63°-67°; lit.1 mp 67°-68°, lit2 mp 66°-68°.

WORKUP

后处理

  1. additionis added dropwise
  2. temperatureto warm to 25° over one hour
  3. customevaporated in vacuo to an oil which
  4. customcrystallizes