HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → 2,3,4,5-Tetrahydro-1H-3-benzazepine--hydrogen chloride (1/1)
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Methanol | HCID 887 | — |
| Reactant | 1H-3-benzazepine-2,4(3H,5H)-dione | HCID 740539 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Product | 2,3,4,5-Tetrahydro-1H-3-benzazepine--hydrogen chloride (1/1) | HCID 17065230 | 78% |
Reaction Steps
To a suspension of 1,5-dihydro-benzo[d]azepine-2,4-dione (9.3 g) in toluene (250 ml) borane-methylsulfide complex (20 ml) was added dropwise under nitrogen atmosphere, then the mixture was heated at reflux for 4 h. MeOH (20 ml) was added dropwise and the mixture refluxed for additional 1 h, then cooled to room temperature. A 10% solution of anidrous HCl in ethyl ether (50 ml) was added and the solid precipitate was filtered off, washed with ethyl ether and desiccated under reduced pressure to afford the title compound as a white solid (7.6 g, 78% yield).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07989444B2 |
| Source dataset | uspto-grants-2011_08 |
| ORD ID | ord-90abf9a9ab5a46259508b58d628e8345 |
| Source note | uspto-grants-2011_08 |