HRID705712
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
- 22.5 °C
PROCEDURE
实验过程
To a mixture of 4-(7-chloro-1,3-benzodioxol-5-yl)-2-pyrimidin-2-yl-5-(trifluoromethyl)pyrazol-3-amine (0.200 g, 0.50 mmol) and NaH (0.015 g, 0.64 mmol) in tetrahydrofurane is added ethylisocyanate (0.078 g, 1.10 mmol). The mixture is refluxed for 4 hours. The reaction was cooled to room temperature (20-25° C.), diluted with water and extracted with ethyl acetate; the organic layer separated and further washed with water and then dried and concentrated. The residue was re-crystallized with a mixture of ethyl acetate and petrole ether to give the title compound (46 mg; 16%).
WORKUP
后处理
- temperatureThe mixture is refluxed for 4 hours
- extractionextracted with ethyl acetate
- customthe organic layer separated
- washfurther washed with water
- customdried
- concentrationconcentrated
- customThe residue was re-crystallized with a mixture of ethyl acetate and petrole ether