反应详情

温度

60 °C

To a mixture of hydroxylamine sulfate (0.59 g, 3.6 mmol) and NaHCO3 (0.700 g, 8.3 mmol) in MeOH (1 mL) and water (10 mL) was added 5-fluoro-4-(fluoromethyl)-4-methyl-3-oxopentanenitrile (0.483 g, 3 mmol). After heated at 60° C. for 8 hours, to it was added 10% HCl until pH 1. It was heated at 60° C. for 3 hours, basified with saturated NaHCO3, and extracted with CH2Cl2. Extracts were dried over MgSO4 and concentrated under reduced pressure to afford 5-(1,3-difluoro-2-methylpropan-2-yl)isoxazol-3-amine as needles (0.289 g, 55%). 1H NMR (300 MHz, CDCl3) δ 5.76 (s, 1H), 4.59 (q, 2H), 4.50 (q and br, 4H), 1.37 (s, 3H); LC-MS (ESI) m/z 177 (M+H)+.

1. temperatureIt was heated at 60° C. for 3 hours
2. extractionextracted with CH2Cl2
3. dry with materialExtracts were dried over MgSO4
4. concentrationconcentrated under reduced pressure