HRID377592

反应详情

EQUATION

反应方程式

HRID 377592 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 6H-indeno[2,1-c]isoquinoline-5,7-dion obtained in reference example 16 (26.6 g, 108 mmol) and phophorous oxychloride (300 ml) was refluxed with heat in the presence of 1 ml of N,N-dimethylformamide for 2 hours. The reaction mixture was distilled to dryness. To the residue was added ice water to obtain a crystal precipitated by filtration. The crystal obtained was washed with water and recrystallized from toluene to give 22.5 g (yield 78.7%) of the title compound.

WORKUP

后处理

  1. temperaturewas refluxed
  2. distillationThe reaction mixture was distilled to dryness
  3. additionTo the residue was added ice water
  4. customto obtain a crystal
  5. customprecipitated by filtration
  6. customThe crystal obtained
  7. washwas washed with water
  8. customrecrystallized from toluene