HRID1168139

反应详情

EQUATION

反应方程式

HRID 1168139 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

58 g of 3-[4-chloro-2,6-difluorophenyl]-1-methyl-6-trifluoromethyl-2,4-(1H,3H)-pyrimidinedione were dissolved in 400 ml of concentrated sulfuric acid and, at 0° C., admixed dropwise with a mixture of 10.7 g of 98% strength nitric acid and 10 ml of concentrated sulfuric acid. The mixture was stirred at 0° C. for 30 minutes and then at 20° C. for 18 hours. Another 10.7 g of the acid mixture were then added dropwise at 0° C. The mixture was stirred at 20° C. for two hours and then poured into ice-water, and the resulting precipitate was filtered off with suction and washed with water until neutral. The solid was dried in a vacuum drying cabinet. Yield: 58.0 g;

WORKUP

后处理

  1. waitat 20° C. for 18 hours
  2. stirringThe mixture was stirred at 20° C. for two hours
  3. filtrationthe resulting precipitate was filtered off with suction
  4. washwashed with water until neutral
  5. customThe solid was dried in a vacuum
  6. customdrying cabinet