HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → 1-[(S)-6-bromo-5-(o-chlorophenyl)-2,3-dihydro-1,3-dimethyl-2-oxo-1H-1,4-benzodiazepin-7-yl]-3-(2,3-dihydroxypropyl)urea
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | 1-[(S)-6-bromo-5-(o-chlorophenyl)-2,3-dihydro-1,3-dimethyl-2-oxo-1H-1,4-benzodiazepin-7-yl]-3-[(2,2-dimethyl-1,3-dioxolan-4-yl)methyl]urea | HCID 54334713 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | 1-[(S)-6-bromo-5-(o-chlorophenyl)-2,3-dihydro-1,3-dimethyl-2-oxo-1H-1,4-benzodiazepin-7-yl]-3-(2,3-dihydroxypropyl)urea | HCID 54119317 | — |
Reaction Steps
A solution of 1-[(S)-6-bromo-5-(o-chlorophenyl)-2,3-dihydro-1,3-dimethyl-2-oxo-1H-1,4-benzodiazepin-7-yl]-3-[(2,2-dimethyl-1,3-dioxolan-4-yl)methyl]urea in ethanol is stirred at room temperature for 5 hours with 1N hydrochloric acid. The mixture is extracted with ethyl acetate, washed with water, dried over sodium sulphate and evaporated. The residue is chromatographed on silica gel while eluting with ethyl acetate/methanol (95:5). After recrystallization from methanol/ether, there is obtained 1-[(S)-6-bromo-5-(o-chlorophenyl)-2,3-dihydro-1,3-dimethyl-2-oxo-1H-1,4-benzodiazepin-7-yl]-3-(2,3-dihydroxypropyl)urea of melting point 175° (decomposition).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04474777 |
| Source dataset | uspto-grants-1984_10 |
| ORD ID | ord-bb78981432d34c2b9a2efde104742cd9 |
| Source note | uspto-grants-1984_10 |