HRID2105206

反应详情

EQUATION

反应方程式

HRID 2105206 的结构方程式

PROCEDURE

实验过程

A mixture of 6-methoxycarbonyl-2-{2-[3-(pyrid-2-yl)isoxazol-5-yl]pyrrolidin-1-yl}-4-(5-methyl-1H-pyrazol-3-ylamino)pyrimidine (Example 56) (200 mg, 0.45 mmol) and a solution of 7N ammonia in methanol (7 ml, 49 mmol) was heated at 65° C. in a sealed vessel under microwave irradiation for 1 hour. The reaction mixture was evaporated, dissolved in methanol and passed through a 50 g isolute SCX-2 ion exchange column. The column was eluted with methanol to elute any neutrals, followed by 7M methanolic ammonia to elute the product. The solvent was removed by evaporation and the residue triturated with diethylether. The resulting solid was collected by filtration to give the title compound (180.0 mg, 93%).

WORKUP

后处理

  1. customThe reaction mixture was evaporated
  2. dissolutiondissolved in methanol
  3. washThe column was eluted with methanol
  4. washto elute any neutrals
  5. washto elute the product
  6. customThe solvent was removed by evaporation
  7. customthe residue triturated with diethylether
  8. filtrationThe resulting solid was collected by filtration