HRID919167

反应详情

EQUATION

反应方程式

HRID 919167 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 2-fluoro-4-(trifluoromethyl)aniline (498 g, 2.783 mmol, 1.00 eq.) in acetonitrile (5 L) was added N-chlorosuccinimide (NCS, 408 g, 3.06 mmol, 1.1 eq.). Then the solution was heated under reflux for 3 hours and then concentrated under vacuum, diluted with petroleum ether (PE 1 L) and filtered. The filtrate was concentrated under vacuum to afford a red oil. The oily product was purified by vacuum distillation to give 2-chloro-6-fluoro-4-(trifluoromethyl)aniline as a yellow liquid (420 g, 71%).

WORKUP

后处理

  1. temperatureThen the solution was heated
  2. temperatureunder reflux for 3 hours
  3. concentrationconcentrated under vacuum
  4. additiondiluted with petroleum ether (PE 1 L)
  5. filtrationfiltered
  6. concentrationThe filtrate was concentrated under vacuum
  7. customto afford a red oil
  8. distillationThe oily product was purified by vacuum distillation