反应详情

To a solution of 2-(2,3-difluoro-6-methoxyphenyl)ethanol (800 mg, 4.25 mmol) in DCM (25 mL) at 0° C. was added 1M BBR3 (17.01 mL, 17.01 mmol) solution and the resulting mixture was allowed to warm to room temp and stir for 4 h. Water (dropwise) was then added and after the bubbling stops mixture was diluted with DCM and washed with water, dried (Na2SO4), filtered and concentrated. The residue was then purified by Biotage (5-50%, EtOAc/hexane) to afford 3,4-difluoro-2-(2-hydroxyethyl)phenol (500 mg, 2.87 mmol, 67.5% yield) as clear viscous oil. 1H NMR (500 MHz, CDCl3) δ 7.85 (br. s., 1H), 7.04-6.93 (m, 1H), 6.71-6.60 (m, 1H), 4.07-4.01 (m, 2H), 3.04-2.95 (m, 2H), 2.38 (br. s., 1H).

1. washwashed with water
2. dry with materialdried (Na2SO4)
3. filtrationfiltered
4. concentrationconcentrated
5. customThe residue was then purified by Biotage (5-50%, EtOAc/hexane)