HRID2120375

反应详情

EQUATION

反应方程式

HRID 2120375 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Sodium 2-propanethiolate (5.66 g) was added to a solution of 2,3-difluoro-6-nitroaniline (10.04 g) in DMF (200 ml). The mixture was stirred at ambient temperature for 16 hours and then diluted with EtOAc (300 ml) and washed with brine (500 ml). The washing was extracted with EtOAc (300 ml). The organic phases were combined, washed with brine (500 ml), dried and volatile material was removed by evaporation to give the title compound (14.1 g) as a solid. NMR: 1.30 (d, 6H), 3.70 (septet, 1H), 6.70 (dd, 1H), 7.26 (s, 2H), 7.80 (dd, 1H); m/z 229.

WORKUP

后处理

  1. washwashed with brine (500 ml)
  2. extractionThe washing was extracted with EtOAc (300 ml)
  3. washwashed with brine (500 ml)
  4. customdried
  5. customvolatile material was removed by evaporation