HRID3154
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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 phosphorous 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
- temperaturewas refluxed
- distillationThe reaction mixture was distilled to dryness
- additionTo the residue was added ice water
- customto obtain a crystal
- customprecipitated by filtration
- customThe crystal obtained
- washwas washed with water
- customrecrystallized from toluene