Reacción #3248

Ecuación de reacción

3-methyl-5H-indeno[2,1-c]quinoline-6,7-dion

phosphorous oxychloride

→

title compound

Rendimiento 73.4%

6-chloro-3-methyl-7H-indeno[2,1-c]quinoline-7-on

Rendimiento 73.4%

Condiciones de reacción

Tratamiento posterior

1. 1
   Temperaturawas refluxed
2. 2
   Temperaturawith heat for 1.5 hours
3. 3
   workup.DISTILLATIONThe reaction mixture was distilled to dryness
4. 4
   workup.ADDITIONTo the residue was added water
5. 5
   Otroto obtain a crystal
6. 6
   Otroprecipitated by filtration
7. 7
   OtroThe crystal obtained
8. 8
   Lavadowas washed with water
9. 9
   workup.DISSOLUTIONdissolved in chloroform
10. 10
    Filtraciónto filter off undissolved substances
11. 11
    OtroRecrystallization from benzene

Procedimiento

A mixture of 3-methyl-5H-indeno[2,1-c]quinoline-6,7-dion obtained in reference example 5 (700 mg, 2.7 mmol) and phosphorous oxychloride (10 ml, 107 mmol) was refluxed with heat for 1.5 hours. The reaction mixture was distilled to dryness. To the residue was added water to obtain a crystal precipitated by filtration. The crystal obtained was washed with water and dissolved in chloroform to filter off undissolved substances. Recrystallization from benzene to give 550 mg (yield 73.4%) of the title compound.

Fuente