HRID240585

反应详情

EQUATION

反应方程式

HRID 240585 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

A 125 mL, single-neck, round-bottomed flask was charged with di-tert-butoxy-N,N-dimethylmethanamine (48.2 ml, 201 mmol), 3-chloro-2,4-difluorobenzoic acid (9.67 g, 50.2 mmol), and DMF (50 ml). The reaction was heated to 80° C. for 48 hours. After cooling to ambient temperature, the reaction was diluted with saturated NaHCO3 and EtOAc. The aqueous phase was extracted with EtOAc, and the combined organic phases were washed with saturated NaHCO3 and brine, dried, filtered and concentrated to provide the desired product as a gold oil.

WORKUP

后处理

  1. temperatureAfter cooling to ambient temperature
  2. extractionThe aqueous phase was extracted with EtOAc
  3. washthe combined organic phases were washed with saturated NaHCO3 and brine
  4. customdried
  5. filtrationfiltered
  6. concentrationconcentrated