HRID1654118

反应详情

EQUATION

反应方程式

HRID 1654118 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
20 °C

PROCEDURE

实验过程

36.8 g of ethyl 4,4,4-trifluoroacetoacetate were mixed in 400 ml of tetrahydrofuran and 9.6 g of sodium hydride were added at 15° C. over 30 minutes. The mixture was stirred at 20° C. for 1 hour and 0.4 g of potassium iodide and 100 ml of acetone were added. 21 g of chloroacetone in 75 ml of tetrahydrofuran were added dropwise over 15 minutes and the mixture was refluxed for 96 hours and then distilled to obtain 24.4 g of the expected product with a boiling point of 65° C. (0.2 mbar).

WORKUP

后处理

  1. temperaturethe mixture was refluxed for 96 hours
  2. distillationdistilled