HRID983835

反应详情

EQUATION

反应方程式

HRID 983835 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
40 °C

PROCEDURE

实验过程

Under an atmosphere of argon, a solution of 4-Amino-6-(2,4-dichloro-phenyl)-2-phenyl-pyrimidine-5-carbonitrile (1.16 g, 0.34 mmol) in THF (6 ml) was added slowly to a suspension of LiAlH4 in THF (3 ml). After stirring for 2 h at 40° C., the reaction mixture was cooled to −20° C. and water (0.6 ml) was added. After 15 min, ethyl acetate was added and the mixture was filtered through Decalite. The organic phase was then separated, washed with water, and dried over sodium sulfate. Purification by flash chromatography (silica gel, methanol, dichloromethane) afforded the title compound, MS: m/e=344.2 (M+), as a light yellow solid (0.446 g, 40%).

WORKUP

后处理

  1. temperaturethe reaction mixture was cooled to −20° C.
  2. waitAfter 15 min
  3. filtrationthe mixture was filtered through Decalite
  4. customThe organic phase was then separated
  5. washwashed with water
  6. dry with materialdried over sodium sulfate
  7. customPurification by flash chromatography (silica gel, methanol, dichloromethane)