HRID1276077

反应详情

EQUATION

反应方程式

HRID 1276077 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
2.5 °C

PROCEDURE

实验过程

40.8 g of 100% nitric acid were added dropwise at from 0 to 5° C. to a solution of 118.9 g of 3-chloro-2-(4-fluorophenyl)-5-trifluoromethylpyridine in 563 ml of 96% sulfuric acid, and the mixture was then stirred at from 0 to 5° C. for 11/2 hours. For work-up, the reaction mixture was poured into 2 l of ice water, and the product was then extracted with ethyl acetate (3×300 ml). The combined organic phases were washed twice with 100 ml of water in each case, dried over sodium sulfate and then evaporated. Yield: 134.5 g (97%) of a colorless oil which crystallized slowly.

WORKUP

后处理

  1. extractionthe product was then extracted with ethyl acetate (3×300 ml)
  2. washThe combined organic phases were washed twice with 100 ml of water in each case
  3. dry with materialdried over sodium sulfate
  4. customevaporated
  5. customYield: 134.5 g (97%) of a colorless oil which crystallized slowly