HRID1243789

反应详情

EQUATION

反应方程式

HRID 1243789 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
-78 °C

PROCEDURE

实验过程

To a solution of cyclopropyl acetylene (10.0 g, 148 mmol) in 50 mL of ethyl ether at −78° C. under argon was added methyllithiium (1.4 M in ethyl ether, 107 mL, 150 mmol). This solution was stirred at −78° C. for 1 h. Methyl chloroformate (12.0 mL, 154 mmol) was added. The reaction mixture was warmed to room temperature in 2 h and was quenched with water. The organic layer was separated. The aqueous layer was extracted with ethyl ether (50 mL×3). The combined organic layer was dried over sodium sulfate and evaporated to give cyclopropyl-propynoic acid methyl ester as a yellow oil (13.25 g, 72%).

WORKUP

后处理

  1. temperatureThe reaction mixture was warmed to room temperature in 2 h
  2. customwas quenched with water
  3. customThe organic layer was separated
  4. extractionThe aqueous layer was extracted with ethyl ether (50 mL×3)
  5. dry with materialThe combined organic layer was dried over sodium sulfate
  6. customevaporated