反应详情

To a solution of 2-(3,4-difluoro-phenyl)-ethanol (1.00 g, 6.33 mmol) in tetrahydrofuran (63.0 mL) at 0° C. was added triethylamine (1.95 mL, 13.9 mmol) followed by methanesulfonyl chloride (0.538 mL, 6.96 mmol). The solution was allowed to warm to room temperature overnight, quenched with water (20 mL), and diluted with ethyl acetate (100 mL). The layers were separated and the aqueous phase was extracted with ethyl acetate (3×25 mL). The combined organic extracts were washed with saturated NaHCO3 (1×20 mL), brine (1×20 mL), dried over MgSO4, filtered, and concentrated to give the title compound. 1H NMR (CDCl3) δ 2.92 (s, 3H), 3.01 (t, J=6.59 Hz, 2H), 4.37–4.40 (m, 2H), 6.94–6.97 (m, 1H), 7.03–7.06 (m, 1H), 7.07–7.15 (m, 1H) ppm. 19F NMR (CDCl3) 8–140.48–, 137.71 ppm.

1. customquenched with water (20 mL)
2. additiondiluted with ethyl acetate (100 mL)
3. customThe layers were separated
4. extractionthe aqueous phase was extracted with ethyl acetate (3×25 mL)
5. washThe combined organic extracts were washed with saturated NaHCO3 (1×20 mL), brine (1×20 mL)
6. dry with materialdried over MgSO4
7. filtrationfiltered
8. concentrationconcentrated