反应详情

温度

50 °C

To a solution of trimethyl[(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)ethynyl]silane (240 g, 1.07 mol) in 1,2-dimethoxyethane (8000 mL) was added (1Z)—N-hydroxyethanimidoyl chloride (120 g, 1.28 mol) and potassium hydrogen carbonate (214.4 g, 2.141 mol). The reaction mixture was heated to 50° C. After 16 hours, the reaction mixture was filtered and concentrated under reduced pressure. The residue was purified via chromatography on silica gel (10% ethyl acetate/hexanes, linear gradient) to afford 3-methyl-4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-5-(trimethylsilyl)isoxazole. MS ESI calc'd. for C13H24BNO3Si [M]+ 281. found 281. 1H NMR (400 MHz, CDCl3) δ 2.39 (s, 3H), 1.31 (s, 12H), 0.37 (s, 9H).

1. filtrationthe reaction mixture was filtered
2. concentrationconcentrated under reduced pressure
3. customThe residue was purified via chromatography on silica gel (10% ethyl acetate/hexanes, linear gradient)