HRID1811542

反应详情

EQUATION

反应方程式

HRID 1811542 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

A solution of the above 5-ethyl-2-(2′-fluoro-4′-methyl-3′-trifluoromethylanilino)phenylacetic acid N,N-dimethyl amide described in Example 3 (0.9 g, 2,4 mmol) in EtOH (25 mL) and 4N NaOH (12 mL) is heated to 80° C. overnight. After cooling, the reaction is concentrated under reduced pressure and diluted with ice cold EtOAc. The pH of the aqueous layer is adjusted to 1-2 with ice cold 2.5 N HCl. The separated organic layer is dried with Na2SO4 and concentrated to a solid. The solid is purified by trituration with an Et2O/hexane mixture to give the title acid, 5-ethyl-2-2′-fluoro-4′-methyl-3′-trifluoromethylanilino)phenylacetic acid.

WORKUP

后处理

  1. temperatureAfter cooling
  2. concentrationthe reaction is concentrated under reduced pressure
  3. additiondiluted with ice cold EtOAc
  4. dry with materialThe separated organic layer is dried with Na2SO4
  5. concentrationconcentrated to a solid
  6. customThe solid is purified by trituration with an Et2O/hexane mixture