تفاعل #3248

معادلة التفاعل

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

phosphorous oxychloride

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title compound

المردود 73.4%

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

المردود 73.4%

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةwas refluxed
2. 2
   درجة الحرارةwith 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
   أخرىto obtain a crystal
6. 6
   أخرىprecipitated by filtration
7. 7
   أخرىThe crystal obtained
8. 8
   غسيلwas washed with water
9. 9
   workup.DISSOLUTIONdissolved in chloroform
10. 10
    ترشيحto filter off undissolved substances
11. 11
    أخرىRecrystallization from benzene

الإجراء التجريبي

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.

المصدر