反应详情

To a mixture of 4-(7-chloro-1,3-benzodioxol-5-yl)-2-pyrimidin-2-yl-5-(trifluoromethyl)pyrazol-3-amine (0.766 g, 2.00 mmol) and NaH (0.054 g, 2.20 mmol) in tetrahydrofuran at 0° C. is added diethyl chlorophosphate (0.414 g, 2.40 mmol). The mixture is allowed to reach room temperature (20-25° C.) and further stirred for 12 hours. The reaction was 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 (125 mg; 12%).

1. customto reach room temperature
2. custom(20-25° C.)
3. extractionextracted with ethyl acetate
4. customthe organic layer separated
5. washfurther washed with water
6. customdried
7. concentrationconcentrated
8. customThe residue was re-crystallized with a mixture of ethyl acetate and petrole ether