HRID1288039

反应详情

EQUATION

反应方程式

HRID 1288039 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

11.4 Parts of 4-bromo-2-fluoroaniline were added to a solution of 10 parts of cyclohexane-1,2-dicarboxylic anhydride in 100 parts of glacial acetic acid and the mixture was stirred for 2 hours. The mixture was refluxed for 20 hours and then poured into 200 parts of ice. The resulting purple crystals were filtered and recrystallized from 70 parts of methanol at -40° C to yield 7.6 parts of lavender crystals of 2-(4-bromo-2-fluorophenyl)-3a,4,5,6,7,7a-hexahydro-1H-isoindole-1,3(2H)-dione melting at 90°-92° C.

WORKUP

后处理

  1. temperatureThe mixture was refluxed for 20 hours
  2. additionpoured into 200 parts of ice
  3. filtrationThe resulting purple crystals were filtered
  4. customrecrystallized from 70 parts of methanol at -40° C