HRID2105203
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
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
- customThe volatiles were removed by evaporation
- dissolutionthe residue dissolved in DCM
- custompurified by chromatography on silica gel eluting with DCM/methanol (100:0 increasing in polarity to 90:10)
- customThe purified product was triturated with diethylether
- filtrationthe resulting solid collected by filtration