HRID1110726

反应详情

EQUATION

反应方程式

HRID 1110726 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

To a solution of 42.1 g (200 mmol) of 3-chloro-2,4,5-trifluorobenzoic acid (E.P.O. No. 0 183 129) in 100 ml of sulfuric acid was added concentrated nitric acid (50 ml) dropwise such that the reaction temperature stayed below 40° C. The reaction mixture was heated at 60° C. for 18 hours, then poured cautiously onto 500 g of ice water. The aqueous solution was extracted with ether, and the ether extracts were washed with water, dried over magnesium sulfate, and concentrated to give 26.5 g of 3-chloro-2,4,5-trifluoro-6-nitrobenzoic acid.

WORKUP

后处理

  1. customstayed below 40° C
  2. extractionThe aqueous solution was extracted with ether
  3. washthe ether extracts were washed with water
  4. dry with materialdried over magnesium sulfate
  5. concentrationconcentrated