Reaktion #3248

Reaktionsgleichung

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

phosphorous oxychloride

→

title compound

Ausbeute 73.4%

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

Ausbeute 73.4%

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturwas refluxed
2. 2
   Temperaturwith 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
   Sonstigeto obtain a crystal
6. 6
   Sonstigeprecipitated by filtration
7. 7
   SonstigeThe crystal obtained
8. 8
   Waschenwas washed with water
9. 9
   workup.DISSOLUTIONdissolved in chloroform
10. 10
    Filtrationto filter off undissolved substances
11. 11
    SonstigeRecrystallization from benzene

Vorschrift

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.

Quelle