HRID705708
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
PROCEDURE
实验过程
To a solution of diisopropyl sulfoxide (0.75 g, 5.6 mmo) in dichloromethane at −60° C. under argon was added dropwise trifluoroacetic anhydride (1.18 g, 5.6 mmol). The solution was stirred for 20 min at this temperature. Then the 4-(7-chloro-1,3-benzodioxol-5-yl)-2-pyrimidin-2-yl-5-(trifluoromethyl)pyrazol-3-amine (0.97 g, 2.5 mmol) was added and the solution stirred at −60° C. for 1 h. The reaction was diluted with aqueous ammonia; 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 (80 mg; 8%).
WORKUP
后处理
- stirringthe solution stirred at −60° C. for 1 h
- customthe organic layer separated
- washfurther washed with water
- customdried
- concentrationconcentrated
- customThe residue was re-crystallized with a mixture of ethyl acetate and petrole ether