HRID2196295

反应详情

EQUATION

反应方程式

HRID 2196295 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

To a solution of 5-(5-bromo-2-fluoro-phenyl)-5-difluoromethyl-2-methyl-morpholin-3-one (659 mg, 1.949 mmol) in 6.6 mL pyridine was added phosphorus pentasulfide (433 mg, 1.949 mmol) and the mixture was heated to 80° C. for 120 minutes. The reaction mixture was cooled to room temperature and partitioned between 0.1 N NaOH and EtOAc. The layers were separated, washed with brine and EtOAc. The combined organic layers were dried over MgSO4.H2O and evaporated to give 704 mg of the title compound as a diastereomeric mixture.

WORKUP

后处理

  1. temperatureThe reaction mixture was cooled to room temperature
  2. custompartitioned between 0.1 N NaOH and EtOAc
  3. customThe layers were separated
  4. washwashed with brine and EtOAc
  5. dry with materialThe combined organic layers were dried over MgSO4.H2O
  6. customevaporated