Reacción #3250

Ecuación de reacción

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

phosphorous oxychloride

→

title compound

Rendimiento 78.7%

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

Rendimiento 78.7%

Disolventes

N,N-dimethylformamide

Condiciones de reacción

Tratamiento posterior

1. 1
   Temperaturawas refluxed
2. 2
   workup.DISTILLATIONThe reaction mixture was distilled to dryness
3. 3
   workup.ADDITIONTo the residue was added ice water
4. 4
   Otroto obtain a crystal
5. 5
   Otroprecipitated by filtration
6. 6
   OtroThe crystal obtained
7. 7
   Lavadowas washed with water
8. 8
   Otrorecrystallized from toluene

Procedimiento

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.

Fuente