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) was added solid NaIO4 (1235 g, 5.8 mol) portionwise at 10-30° C. Upon completion of the addition, the reaction was stirred 1 h at 15° C. and overnight at rt. The solid precipitate was filtered off and washed with DCM (1 L×2). The organic layer was washed with water (500 mL×2) and brine (500 mL), dried over Na2SO4, and concentrated to provide the title compound as a crude dark solid (238 g, 86.3%), LRMS (M+H+) m/z 191.1.

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