反应详情

温度

60 °C

To a solution of hydroxylamine hydrochloride (60.0 g, 0.86 mol) in water (2 L) was added (E)-3-hydroxy-2-(2-(methylthio)pyrimidin-4-yl)acrylaldehyde (3) (342 g, 0.714 mol) in portions. After the addition, the mixture was heated at 60° C. and stirred for 2 h. The reaction mixture was allowed to cool to room temperature and the solution was adjusted to pH about 4 by addition of 10% aq. NaHCO3. The resulting precipitate was filtered, washed with water (200 mL×2) and dried in vacuum to give 4-(isoxazol-4-yl)-2-(methylthio)pyrimidine (4) (112 g, 81.2%) as a yellow solid.

1. additionAfter the addition
2. temperatureto cool to room temperature
3. filtrationThe resulting precipitate was filtered
4. washwashed with water (200 mL×2)
5. customdried in vacuum