반응 #4134

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4,9-dibromo-6-(4-methyl-1-piperazinyl)-1,2-dihydrobenzo[b]pyrrolo[3,2,1-jk][1,4]-benzodiazepine

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product

수율 75.2%

4,9-Dibromo-6-(4-methyl-1-piperazinyl)benzo[b]pyrrolo[3,2,1-jk][1,4]benzodiazepine

수율 75.2%

용매

chloroform

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후처리

1. 1
   온도under reflux for 3.5 hours
2. 2
   여과The mixture was filtered through celite
3. 3
   농축the filtrate was concentrated
4. 4
   기타The residue was purified by flash chromatography over a silica gel column (140 gm)
5. 5
   세척eluted with 2% methanol
6. 6
   기타The appropriate fractions were collected
7. 7
   기타evaporated
8. 8
   기타Crystallization of the residue from isopropanol (10 ml)

실험 절차

A mixture 4,9-dibromo-6-(4-methyl-1-piperazinyl)-1,2-dihydrobenzo[b]pyrrolo[3,2,1-jk][1,4]-benzodiazepine (4.5 g, 9.45 mmoles) and manganese(IV) dioxide (7.0 g) in chloroform (150 ml) was heated under reflux for 3.5 hours. An additional 4.5 g of manganese dioxide was added. The reaction mixture was stirred overnight at room temperature. The mixture was filtered through celite and the filtrate was concentrated. The residue was purified by flash chromatography over a silica gel column (140 gm), eluted with 2% methanol:98% dichloromethane (2 l). The appropriate fractions were collected and evaporated. Crystallization of the residue from isopropanol (10 ml) yielded 3.37 g (75%) of product, mp 158°-159° C.

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