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
- 45 °C
PROCEDURE
实验过程
To a mixture of [1-amino-1-[4-({(5-chloromethoxy-1-pyrimidin-2-yl-1H-[1,2,4]triazol-3-yl)-[2-fluoro-3-(2-hydroxyethoxy)-5-methoxyphenyl]methyl}amino)phenyl]methylidene]carbamic acid 2,2-dimethylpropyl ester (Example 2b, 100 mg), potassium hydrogen carbonate (109 mg), and DMF (13.3 mL), 2-ethylbutanoic acid (88.3 mg) and sodium iodide (117 mg) were added, and the resulting mixture was stirred at 45° C. overnight and then cooled to room temperature. To the reaction mixture, ice and saturated aqueous ammonium chloride solution were added, and the resulting mixture was extracted with a mixture of THF and ethyl acetate. The organic layer was washed with saturated aqueous ammonium chloride solution and dried over anhydrous magnesium sulfate.
WORKUP
后处理
- additionwere added
- temperaturecooled to room temperature
- extractionthe resulting mixture was extracted with a mixture of THF and ethyl acetate
- washThe organic layer was washed with saturated aqueous ammonium chloride solution
- dry with materialdried over anhydrous magnesium sulfate