反应详情

温度

15 °C

To a mixture of 1-(3-fluoropyridin-2-yl)-3-methylenecyclobutanecarbonitrile (272 g, 1.45 mol) and RuCl3.H2O (9.0 g, 0.044 mol) in DCM (1 L), acetonitrile (1 L), and water (1.5 L) mixture was added solid NaIO4 (1235 g, 5.8 mol) portionwise at 10-30° C. Upon the completion of addition, the reaction was stirred 1 h at 15° C. and overnight at rt. The solid precipitate was filtered off and washed with DCM (2×1000 mL). The organic layer was washed with water (2×500 mL) and brine (500 mL), dried over Na2SO4, and concentrated to provide a crude title compound as a dark solid (238 g), m/z=191.1 [M+H].

1. additionUpon the completion of addition
2. filtrationThe solid precipitate was filtered off
3. washwashed with DCM (2×1000 mL)
4. washThe organic layer was washed with water (2×500 mL) and brine (500 mL)
5. dry with materialdried over Na2SO4
6. concentrationconcentrated