HRID52430

反应详情

EQUATION

反应方程式

HRID 52430 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
-3 °C

PROCEDURE

实验过程

A mixture of N-(4-chloro-2-fluorophenyl)-1-cyclohexene-1,2-dicarboximide (24.4 g, 86.7 mmol) in sulfuric acid (150 mL) is cooled to -3° C., treated dropwise with nitric acid (70% real, 6.70 mL, 104 mmol) while maintaining the temperature at 0°-2° C., stirred at room temperature for 90 minutes, and poured onto ice. The aqueous mixture is stirred for several minutes, and filtered to obtain a solid which is washed with water and dried to give the title product as a white powder (28.6 g, mp 152°-155° C.).

WORKUP

后处理

  1. temperaturewhile maintaining the temperature at 0°-2° C.
  2. additionpoured onto ice
  3. stirringThe aqueous mixture is stirred for several minutes
  4. filtrationfiltered
  5. customto obtain a solid which
  6. washis washed with water
  7. customdried