Reacción #4109

Ecuación de reacción

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

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product

Rendimiento 63.7%

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

Rendimiento 63.7%

Disolventes

chloroform

Condiciones de reacción

Tratamiento posterior

1. 1
   TemperaturaThe mixture was heated
2. 2
   Temperaturaunder reflux for 24 hours
3. 3
   TemperaturaThe mixture was cooled
4. 4
   Filtraciónfiltered
5. 5
   Lavadothe solid was washed with dichloromethane (200 ml)
6. 6
   ConcentraciónThe filtrate was then concentrated to dryness
7. 7
   OtroThe residue was purified by flash chromatography over a silica gel column (150 g)
8. 8
   Lavadoeluted with 2% methanol in dichloromethane (4 l) and 3% methanol in dichloromethane (2 l)
9. 9
   OtroEvaporation of the eluent

Procedimiento

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.

Fuente