HRID2105203

反应详情

EQUATION

反应方程式

HRID 2105203 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
65 °C

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) (62.5 mg, 0.14 mmol), 2N solution of methylamine in methanol (2.0 ml, 4.00 mmol) and methanol (3.0 ml) was heated at 65° C. for 1 hour under microwave irradiation. The volatiles were removed by evaporation and the residue dissolved in DCM and purified by chromatography on silica gel eluting with DCM/methanol (100:0 increasing in polarity to 90:10). The purified product was triturated with diethylether and the resulting solid collected by filtration to give the title compound (21 mg, 34%).

WORKUP

后处理

  1. customThe volatiles were removed by evaporation
  2. dissolutionthe residue dissolved in DCM
  3. custompurified by chromatography on silica gel eluting with DCM/methanol (100:0 increasing in polarity to 90:10)
  4. customThe purified product was triturated with diethylether
  5. filtrationthe resulting solid collected by filtration