HuagongsheHuagongshe Chemistry Print Report · For research reference only
Bromine → HCID 22105470, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Bromine | HCID 24408 | — |
| Reactant | HCID 22105467 | HCID 22105467 | — |
| Solvent | Carbon Tetrachloride | HCID 5943 | — |
| Product | HCID 22105470 | HCID 22105470 | 65.3% |
Reaction Steps
A suspension of 0.78 g (2.56 mmole) of 7-chloro-5-(2-chlorophenyl)-1,3-dihydro-2H-1-benzazepin-2-one in 100 mL of carbon tetrachloride was heated to reflux, yielding a clear solution. Bromine (0.19 mL, 3.69 mmole) was added in one portion and the solution was, heated at reflux, under a sunlamp, for 15 minutes. Without cooling, the reaction solution was washed with 5% aqueous sodium thiosulfate and water, dried (sodium sulfate), and concentrated. The residue was triturated with ether. The solid was collected on a filter, washed with ether and dried yielding 0.64 g (65%) of the title compound. This crude material (shown by NMR to have a ratio of product to starting material of 85:15) was used as is in the next step.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05843941 |
| Source dataset | uspto-grants-1998_12 |
| ORD ID | ord-53b8f6bbca1244dfb46cb171cd26728e |
| Source note | uspto-grants-1998_12 |