Réaction #3250

Équation de réaction

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

phosphorous oxychloride

→

title compound

Rendement 78.7%

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

Rendement 78.7%

Solvants

N,N-dimethylformamide

Conditions de réaction

Traitement

1. 1
   Températurewas refluxed
2. 2
   workup.DISTILLATIONThe reaction mixture was distilled to dryness
3. 3
   workup.ADDITIONTo the residue was added ice water
4. 4
   Autreto obtain a crystal
5. 5
   Autreprecipitated by filtration
6. 6
   AutreThe crystal obtained
7. 7
   Lavagewas washed with water
8. 8
   Autrerecrystallized from toluene

Mode opératoire

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.

Source