HRID1429582
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
To a solution of 6-bromo-2-(piperidin-4-yloxy)benzo[d]thiazole (1 g, 3.19 mmol) and 2-chloro-5-fluoropyrimidine (0.508 g, 3.83 mmol) in DMF (15 mL) was added potassium carbonate (1.32 g, 9.58 mmol). The reaction mixture was stirred at 100° C. for 4 h. The reaction mixture was cooled to rt, diluted with water (40 mL), and extracted with EtOAc (3×20 mL). The combined organic layers were dried (Na2SO4), filtered, and concentrated. The residue was purified by column chromatography (silica gel, hexanes-EtOAc gradient 0 to 40% EtOAc) to afford 6-bromo-2-(1-(5-fluoropyrimidin-2-yl)piperidin-4-yloxy)benzo[d]thiazole (1.112 g, 2.72 mmol, 85% yield) as a white solid.
WORKUP
后处理
- temperatureThe reaction mixture was cooled to rt
- extractionextracted with EtOAc (3×20 mL)
- dry with materialThe combined organic layers were dried (Na2SO4)
- filtrationfiltered
- concentrationconcentrated
- customThe residue was purified by column chromatography (silica gel, hexanes-EtOAc gradient 0 to 40% EtOAc)