HuagongsheHuagongshe Chemistry Print Report · For research reference only
Boron tribromide → N-Trifluoroacetyl-8-bromo-7-hydroxy-1-isopropyl-2,3,4,5-tetrahydro-1H-3-benzazepine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Boron tribromide | HCID 25134 | — |
| Reactant | N-trifluoroacetyl-8-bromo-1-isopropyl-7-methoxy-2,3,4,5-tetrahydro-1H-3-benzazepine | HCID 22292805 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | N-Trifluoroacetyl-8-bromo-7-hydroxy-1-isopropyl-2,3,4,5-tetrahydro-1H-3-benzazepine | HCID 22292823 | 97.3% |
Reaction Steps
A solution of N-trifluoroacetyl-8-bromo-1-isopropyl-7-methoxy-2,3,4,5-tetrahydro-1H-3-benzazepine (0.041 g, 0.10 mmol) in dichloromethane (1 mL) was treated with BBr3 (0.32 ml, 1.0 M solution in CH2Cl2) and stirred overnight at 20 C. The excess BBr3 is quenched with water and the resulting mixture diluted with ether (50 mL), washed twice with saturated aqueous Na2CO3 (20 mL) and concentrated. Flash chromatography (20% EtOAc in hexanes, silica) resulted in 0.037 g clear oil. MS calculated for C15H17BrF3NO2+H: 380, observed: 380.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08993750B2 |
| Source dataset | uspto-grants-2015_03 |
| ORD ID | ord-f86cc930e4394716ba24ab87282fa2f7 |
| Source note | uspto-grants-2015_03 |