HRID1090860

反应详情

EQUATION

反应方程式

HRID 1090860 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

200 ml of tetrahydrofuran and 50 g of 2,4,6-trifluorobenzotrifluoride were initially introduced into a stainless steel autoclave and it was pressurized using 30 ml of liquid ammonia. Subsequently, the mixture was heated at 120° C. for 6 hours with stirring. After cooling and releasing the pressure, the reaction mixture was subjected to a fractional distillation. 15 g of 2-amino-4,6-difluoro-benzotrifluoride were obtained at a boiling point of 57° to 58° C. at 12 mbar. After a small intermediate run, 32 g of 2,6-difluoro-4-amino-benzotrifluoride passed over at a boiling point of 103° to 105° C. at 16 mbar. The melting point of the 2,6-difluoro-4-amino-benzotrifluoride obtained was 66° C.

WORKUP

后处理

  1. temperatureAfter cooling
  2. distillationthe reaction mixture was subjected to a fractional distillation