تفاعل #3250

معادلة التفاعل

6H-indeno[2,1-c]isoquinoline-5,7-dion

phosphorous oxychloride

→

title compound

المردود 78.7%

5-chloro-7H-indeno[2,1-c]isoquinoline-7-on

المردود 78.7%

المذيبات

N,N-dimethylformamide

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةwas refluxed
2. 2
   workup.DISTILLATIONThe reaction mixture was distilled to dryness
3. 3
   workup.ADDITIONTo the residue was added ice water
4. 4
   أخرىto obtain a crystal
5. 5
   أخرىprecipitated by filtration
6. 6
   أخرىThe crystal obtained
7. 7
   غسيلwas washed with water
8. 8
   أخرىrecrystallized from toluene

الإجراء التجريبي

A mixture of 6H-indeno[2,1-c]isoquinoline-5,7-dion obtained in reference example 16 (26.6 g, 108 mmol) and phosphorous oxychloride (300 ml) was refluxed with heat in the presence of 1 ml of N,N-dimethylformamide for 2 hours. The reaction mixture was distilled to dryness. To the residue was added ice water to obtain a crystal precipitated by filtration. The crystal obtained was washed with water and recrystallized from toluene to give 22.5 g (yield 78.7%) of the title compound.

المصدر