HuagongsheHuagongshe Chemistry Print Report · For research reference only
4-Chloro-6-(4-methyl-1-piperazinyl)-1,2,dihydrobenzo[b]pyrrolo[3,2,1-jk][1,4]benzodiazepine → 4-Chloro-6-(4-methyl-1-piperazinyl)benzo[b]pyrrolo[3,2,1-jk]-[1,4]benzodiazepine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 4-Chloro-6-(4-methyl-1-piperazinyl)-1,2,dihydrobenzo[b]pyrrolo[3,2,1-jk][1,4]benzodiazepine | HCID 13823295 | — |
| Catalyst | HCID 178418406 | HCID 178418406 | — |
| Solvent | Chloroform | HCID 6212 | — |
| Product | 4-Chloro-6-(4-methyl-1-piperazinyl)benzo[b]pyrrolo[3,2,1-jk]-[1,4]benzodiazepine | HCID 13823301 | 63.7% |
Reaction Steps
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.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04723003 |
| Source dataset | uspto-grants-1988_02 |
| ORD ID | ord-e9900028a3e64abb947a008cb915a7e1 |
| Source note | uspto-grants-1988_02 |