2-Bromophenol → HCID 15058601, compound

To a solution of 2-bromophenol (1.0 g, 5.8 mmol) in THF (20 mL) was add NaH (60%) (462 mg, 11.6 mmol). The reaction mixture was stirred at room temperature for 10 min and then 1-bromo-2-fluoroethane (1.5 g, 11.6 mmol) was added and the mixture was irradiated in a microwave reactor at 130° C. for 40 min. The crude mixture was quenched with H2O and the water layer was extracted with EtOAc. The combined organic layers were dried (Na2SO4), filtered and concentrated. The residue was purified by chromatography on silica gel (0-20% DCM in Heptane) to provide the desired compound as a colorless oil (800 mg, 63%).

1. customthe mixture was irradiated in a microwave reactor at 130° C. for 40 min
2. customThe crude mixture was quenched with H2O
3. extractionthe water layer was extracted with EtOAc
4. dry with materialThe combined organic layers were dried (Na2SO4)
5. filtrationfiltered
6. concentrationconcentrated
7. customThe residue was purified by chromatography on silica gel (0-20% DCM in Heptane)

ORD record

ord-d786827193f744f194c191ffa33e82b8

Source dataset

uspto-grants-2015_06

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09066946B2