HRID509121
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
- 120 °C
PROCEDURE
实验过程
A mixture of 2-chloropyrimidine (1.37 g, 12 mmol), 2,4-dimethoxybenzylamine (2.61 g, 15.6 mmol) and triethylamine (2.51 mL, 18 mmol) in ethanol (8 mL) was heated in the microwave at 120° C. for 15 minutes. Water was added to the reaction mixture and the mixture extracted with dichloromethane (×3). The combined organic layers were washed with brine, dried over magnesium sulfate and concentrated in vacuo. The residue was purified using silica gel column chromatography (20-50% ethyl acetate in heptane gradient elution) to afford the title compound as a white solid (2.14 g, 72%).
WORKUP
后处理
- extractionthe mixture extracted with dichloromethane (×3)
- washThe combined organic layers were washed with brine
- dry with materialdried over magnesium sulfate
- concentrationconcentrated in vacuo
- customThe residue was purified
- washsilica gel column chromatography (20-50% ethyl acetate in heptane gradient elution)