Réaction #4109

Équation de réaction

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

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product

Rendement 63.7%

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

Rendement 63.7%

Solvants

chloroform

Conditions de réaction

Traitement

1. 1
   TempératureThe mixture was heated
2. 2
   Températureunder reflux for 24 hours
3. 3
   TempératureThe mixture was cooled
4. 4
   Filtrationfiltered
5. 5
   Lavagethe solid was washed with dichloromethane (200 ml)
6. 6
   ConcentrationThe filtrate was then concentrated to dryness
7. 7
   AutreThe residue was purified by flash chromatography over a silica gel column (150 g)
8. 8
   Lavageeluted with 2% methanol in dichloromethane (4 l) and 3% methanol in dichloromethane (2 l)
9. 9
   AutreEvaporation of the eluent

Mode opératoire

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 l) and 3% methanol in dichloromethane (2 l). Evaporation of the eluent gave 3.8 g (63%) of product. Recrystallization from toluene (40 ml) yielded the analytical sample, mp 170°-172° C.

Source