HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonium Chloride → 10-Bromo-5,6-dihydroimidazo[1,2-d][1,4]benzoxazepine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | 10-Bromo-2-iodo-5,6-dihydrobenzo[F]imidazo[1,2-D][1,4]oxazepine | HCID 58204407 | — |
| Reactant | HCID 178418443 | HCID 178418443 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 10-Bromo-5,6-dihydroimidazo[1,2-d][1,4]benzoxazepine | HCID 58204739 | — |
Reaction Steps
To a solution of 10-bromo-2-iodo-5,6-dihydrobenzo[f]imidazo[1,2-d][1,4]oxazepine (9 g, 20 mmol) in THF (40 mL) was added Ethylmagnesium bromide in Ethyl ether (22 mL) at −20° C. The mixture was allowed to warm to room temperature and in one and half hour the completion was showed by LCMS. The reaction mixture was poured into 10% NH4Cl and extracted by EtOAc. Organic layer was washed by brine, dried by MgSO4 and concentrated. The crude was purified by Isco chromatography to afford 10-bromo-5,6-dihydrobenzo[f]imidazo[1,2-d][1,4]oxazepine. LC/MS (ESI+): m/z 265 (M+H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08242104B2 |
| Source dataset | uspto-grants-2012_08 |
| ORD ID | ord-850abbe392214bf29f2fe6ad9ca35ce6 |
| Source note | uspto-grants-2012_08 |