HRID705707

反应详情

EQUATION

反应方程式

HRID 705707 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of diethyl sulfoxide (0.47 g, 4.4 mmo) in dichloromethane at −60° C. under argon was added drop-wise trifluoroacetic anhydride (0.93 g, 4.4 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 (0.76 g, 2 mmol) was added and the solution stirred at −60 C for 1 h. The reaction was diluted with aqueous ammonia; the organic layer was 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 (270 mg; 29%).

WORKUP

后处理

  1. stirringthe solution stirred at −60 C for 1 h
  2. customthe organic layer was separated
  3. washfurther washed with water
  4. customdried
  5. concentrationconcentrated
  6. customThe residue was re-crystallized with a mixture of ethyl acetate and petrole ether