반응 #3248

반응 방정식

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

phosphorous oxychloride

→

title compound

수율 73.4%

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

수율 73.4%

반응 조건

후처리

1. 1
   온도was refluxed
2. 2
   온도with 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
   기타to obtain a crystal
6. 6
   기타precipitated by filtration
7. 7
   기타The crystal obtained
8. 8
   세척was washed with water
9. 9
   workup.DISSOLUTIONdissolved in chloroform
10. 10
    여과to filter off undissolved substances
11. 11
    기타Recrystallization from benzene

실험 절차

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.

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