HRID983835
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturethe reaction mixture was cooled to −20° C.
- waitAfter 15 min
- filtrationthe mixture was filtered through Decalite
- customThe organic phase was then separated
- washwashed with water
- dry with materialdried over sodium sulfate
- customPurification by flash chromatography (silica gel, methanol, dichloromethane)