تفاعل #62639

معادلة التفاعل

4-chloro-6-(4-methyl-1-piperazinyl)-1,2,-dihydrobenzo[b]pyrrolo[3,2,1-jk][1,4]benzodiazepine

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product

المردود 63.7%

4-Chloro-6-(4-methyl-1-piperazinyl)benzo[b]pyrrolo[3,2,1-jk]-[1,4]benzodiazepine

المردود 63.7%

المذيبات

chloroform

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةThe mixture was heated
2. 2
   درجة الحرارةunder reflux for 24 hours
3. 3
   درجة الحرارةThe mixture was cooled
4. 4
   ترشيحfiltered
5. 5
   غسيلthe solid was washed with dichloromethane (200 ml)
6. 6
   تركيزThe filtrate was then concentrated to dryness
7. 7
   أخرىThe residue was purified by flash chromatography over a silica gel column (150 g)
8. 8
   غسيلeluted with 2% methanol in dichloromethane (4 1) and 3% methanol in dichloromethane (2 1)
9. 9
   أخرىEvaporation of the eluent

الإجراء التجريبي

To a solution of 4-chloro-6-(4-methyl-1-piperazinyl)-1,2,-dihydrobenzo[b]pyrrolo[3,2,1-jk][1,4]benzodiazepine (6 g, 17 mmoles), in chloroform (150 ml) was added manganese dioxide (10.5 g). The mixture was heated under reflux for 24 hours. The mixture was cooled, filtered and the solid was washed with dichloromethane (200 ml). The filtrate was then concentrated to dryness. The residue was purified by flash chromatography over a silica gel column (150 g), eluted with 2% methanol in dichloromethane (4 1) and 3% methanol in dichloromethane (2 1). Evaporation of the eluent gave 3.8 g (63%) of product. Recrystallization from toluene (40 ml) yielded the analytical sample, mp 170°-172° C.

المصدر