HRID2196338

反应详情

EQUATION

反应方程式

HRID 2196338 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
68 °C

PROCEDURE

实验过程

A mixture of 5-difluoromethyl-5-(2-fluoro-phenyl)-morpholin-3-one (141 g, 575 mmol) and Lawesson's reagent (132 g, 316 mmol) in 1400 ml of THF was heated at 68° C. for 1 h, cooled down and then evaporated. The residue was dissolved in 1 L DCM and filtered over 2 Kg silica gel with 10 L DCM to give 161 g of the title compound in the form of a greenish resin that slowly crystallized. The compound was used without further purification.

WORKUP

后处理

  1. temperaturecooled down
  2. customevaporated
  3. dissolutionThe residue was dissolved in 1 L DCM
  4. filtrationfiltered over 2 Kg silica gel with 10 L DCM