反応 #3250

反応方程式

6H-indeno[2,1-c]isoquinoline-5,7-dion

phosphorous oxychloride

→

title compound

収率 78.7%

5-chloro-7H-indeno[2,1-c]isoquinoline-7-on

収率 78.7%

溶媒

N,N-dimethylformamide

反応条件

後処理

1. 1
   温度was refluxed
2. 2
   workup.DISTILLATIONThe reaction mixture was distilled to dryness
3. 3
   workup.ADDITIONTo the residue was added ice water
4. 4
   その他to obtain a crystal
5. 5
   その他precipitated by filtration
6. 6
   その他The crystal obtained
7. 7
   洗浄was washed with water
8. 8
   その他recrystallized from toluene

実験手順

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.

出典