HuagongsheHuagongshe Chemistry Print Report · For research reference only
Nitrobenzene → 2-oxo-3-tert-butoxycarbonylamino-5-phenyl-8-methyl-1,3,4,5-tetrahydro-2H-1,5-benzodiazepine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Nitrobenzene | HCID 7416 | — |
| Reactant | 2-oxo-3-tert-butoxycarbonylamino-5-(2-cyclohexene-1-yl)-8-methyl-1,3,4,5-tetrahydro-2H-1,5-benzodiazepine | HCID 21201541 | — |
| Catalyst | HCID 178418390 | HCID 178418390 | — |
| Solvent | O-Xylene | HCID 7237 | — |
| Product | 2-oxo-3-tert-butoxycarbonylamino-5-phenyl-8-methyl-1,3,4,5-tetrahydro-2H-1,5-benzodiazepine | HCID 21201770 | 83.5% |
Reaction Steps
2-Oxo-3-tert-butoxycarbonylamino-5-(2-cyclohexen-1-yl)-8-methyl-1,3,4,5-tetrahydro-2H-1,5-benzodiazepine (500 mg) was suspended in xylene (20 ml), nitrobenzene (831 mg) and 10% palladium carbon (250 mg) were added therto, and the mixture was refluxed for 2 hours. The reaction mixture was allowed to cool, filtrated, and the filtrate was concentrated under reduced pressure. Diisopropyl ether was added to the residue, crystals so precipitated were collected by filtration, to thereby obtain 413 mg of the titled compound (Yield: 83%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06239131B1 |
| Source dataset | uspto-grants-2001_05 |
| ORD ID | ord-9ab8b04b09084eb4acce0b6b02ef6938 |
| Source note | uspto-grants-2001_05 |