HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Hydroxide → HCID 10567395, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 10545524 | HCID 10545524 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | HCID 10567395 | HCID 10567395 | 82.8% |
Reaction Steps
4,4-Difluoro-1-(4-nitrobenzoyl)-2,3,4,5-tetrahydro-1H-1-benzazepin-5-one (940 mg) was dissolved in 20 ml of acetic acid, 3.07 g of stannous chloride was added to the solution at room temperature and then the resulting mixture was heated under reflux for 5 hours. The reaction solution was ice-cooled and adjusted to a basic range with 1N sodium hydroxide. Then, after separating the organic layer, the water layer was extracted with ethyl acetate. The resulting organic layer was dried over anhydrous potassium carbonate and the solvent was evaporated under a reduced pressure. The thus prepared residue was recrystallized from chloroformhexane to obtain 711 mg of 1-(4-aminobenzoyl)-4,4-difluoro-2,3,4,5-tetrahydro-1H-1-benzazepin-5-one.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05710150 |
| Source dataset | uspto-grants-1998_01 |
| ORD ID | ord-652ded4a9c774e0bafb8ac9254830fb4 |
| Source note | uspto-grants-1998_01 |