Реакция #3248

Уравнение реакции

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

phosphorous oxychloride

→

title compound

Выход 73.4%

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

Выход 73.4%

Условия реакции

Обработка

1. 1
   Температураwas refluxed
2. 2
   Температураwith 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
   Другоеto obtain a crystal
6. 6
   Другоеprecipitated by filtration
7. 7
   ДругоеThe crystal obtained
8. 8
   Промывкаwas washed with water
9. 9
   workup.DISSOLUTIONdissolved in chloroform
10. 10
    Фильтрацияto filter off undissolved substances
11. 11
    ДругоеRecrystallization from benzene

Методика

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.

Источник