HRID705712

反应详情

EQUATION

反应方程式

HRID 705712 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureThe mixture is refluxed for 4 hours
  2. extractionextracted with ethyl acetate
  3. customthe organic layer separated
  4. washfurther washed with water
  5. customdried
  6. concentrationconcentrated
  7. customThe residue was re-crystallized with a mixture of ethyl acetate and petrole ether