反応 #3248

反応方程式

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

phosphorous oxychloride

→

title compound

収率 73.4%

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

収率 73.4%

反応条件

後処理

1. 1
   温度was refluxed
2. 2
   温度with 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
   その他to obtain a crystal
6. 6
   その他precipitated by filtration
7. 7
   その他The crystal obtained
8. 8
   洗浄was washed with water
9. 9
   workup.DISSOLUTIONdissolved in chloroform
10. 10
    ろ過to filter off undissolved substances
11. 11
    その他Recrystallization from benzene

実験手順

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.

出典