Hydrogen Bromide → Methyl 2-bromo-2-(3-fluorophenyl)acetate
Reaction equation
[F:1][C:2]1[CH:3]=[C:4]([CH2:8][C:9]([O:11][CH3:12])=[O:10])[CH:5]=[CH:6][CH:7]=1.[Br:13]N1C(=O)CCC1=O.Br>C(Cl)(Cl)(Cl)Cl.C(Cl)Cl>[Br:13][CH:8]([C:4]1[CH:5]=[CH:6][CH:7]=[C:2]([F:1])[CH:3]=1)[C:9]([O:11][CH3:12])=[O:10]Participants
6
Procedure
Methyl 2-(3-fluorophenyl)acetate (1.90 g, 11.3 mmol) and N-bromo succinimide (2.01 g, 11.3 mmol) were dissolved in CCl4 (80 ml). HBr (64 ul, 0.56 mmol) was added, and the mixture was stirred under reflux overnight. The mixture was cooled at room temperature, diluted with DCM, and washed with sat. NaHCO3, water and brine. The organic layer was dried (Na2SO4), filtered, and evaporated obtaining intermediate I15 (2.68 g, 96% yield).
Workup
- temperatureunder reflux overnight
- washwashed with sat. NaHCO3, water and brine
- dry with materialThe organic layer was dried (Na2SO4)
- filtrationfiltered
- customevaporated
- customobtaining intermediate I15 (2.68 g, 96% yield)
Sources & evidence
- ORD record
- ord-6feb96ab08bc4bf7ae345ccae01b3d8c
- Source dataset
- uspto-grants-2013_10
- Patent number
- US08563577B2
Reaction notes
Loading…