反応 #4192

反応方程式

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

収率 75.2%

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

収率 75.2%

溶媒

chloroform

反応条件

後処理

1. 1
   温度under reflux for 3.5 hours
2. 2
   ろ過The mixture was filtered through celite
3. 3
   濃縮the filtrate was concentrated
4. 4
   その他The residue was purified by flash chromatography over a silica gel column (140 gm)
5. 5
   洗浄eluted with 2% methanol
6. 6
   その他The appropriate fractions were collected
7. 7
   その他evaporated
8. 8
   その他Crystallization of the residue from isopropanol (10 ml)

実験手順

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.

出典