HRID592409
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
- 100 °C
PROCEDURE
实验过程
A mixture of 1-isopropylpyrazol-4-amine (0.083 g, 0.66 mmol), 1-(2-(2-(2,5-dichloropyrimidin-4-yl)ethyl)phenyl)cyclopropanecarboxamide A14 (0.110 g, 0.327 mmol) and TsOH.H2O (0.013 g, 0.066 mmol) in 1,4-dioxane (2.0 mL) was heated in the microwave to 100° C. for 3 hours. The mixture was concentrated under reduced pressure and purified by silica gel column chromatography (0-100% EtOAc in petroleum benzine 40-60° C. then 0-10% MeOH in EtOAc) to give the title compound 30 (0.094 g, 68%). LCMS-D: rt 3.355 min; m/z 425.3 [M+H]+.
WORKUP
后处理
- concentrationThe mixture was concentrated under reduced pressure
- custompurified by silica gel column chromatography (0-100% EtOAc in petroleum benzine 40-60° C.