Reaktion #4187

Reaktionsgleichung

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

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product

Ausbeute 42.7%

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

Ausbeute 42.7%

Lösungsmittel

chloroform

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturthe mixture was heated
2. 2
   Temperaturunder reflux for 4 days
3. 3
   FiltrationThe mixture was filtered
4. 4
   Waschenthe filter cake washed with dichloromethane
5. 5
   EinengenThe filtrate was concentrated under vacuum
6. 6
   SonstigeThe residue was purified on a silica gel column
7. 7
   Wascheneluted with 2% methanol/dichloromethane
8. 8
   workup.ADDITIONThe fractions (75-100 ml each) containing pure product
9. 9
   Einengenconcentrated
10. 10
    SonstigeRecrystallization from a small volume of 2-propanol

Vorschrift

To a solution of 4-bromo-6-(4-methyl-1-piperazinyl)-9-methyl-1,2-dihydrobenzo[b]pyrrolo[3,2,1-jk][1,4]benzodiazepine (5.7 g, 13.8 mmoles) in chloroform (540 ml) was added manganese dioxide (25 gm), and the mixture was heated under reflux for 4 days. The mixture was filtered, and the filter cake washed with dichloromethane. The filtrate was concentrated under vacuum. The residue was purified on a silica gel column, eluted with 2% methanol/dichloromethane. The fractions (75-100 ml each) containing pure product were pooled and concentrated. Recrystallization from a small volume of 2-propanol yielded 2.41 g (42%) of product, mp 153°-155° C.

Quelle