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
PROCEDURE
实验过程
To a mixture of 0.44 g of 1-butanol and 6 ml of DMF was added 0.24 g of 60% sodium hydride (oily) under ice cool, and the mixture was stirred for 10 minutes. And, 2-(3-fluoropyridin-4-yl-)-1-methyl-5-trifluoromethyl-1H-benzimidazole (0.35 g) was added, then, the mixture was stirred for 1.5 hours at room temperature. Into the reaction mixture was poured a saturated ammonium chloride aqueous solution, and the mixture was extracted three times with ethyl acetate. The organic layer was dried over magnesium sulfate, then, concentrated under reduced pressure. The residue was subjected to silica gel column chromatography, to obtain 0.37 g of 2-(3-butoxypyridin-4-yl-)-1-methyl-5-trifluoromethyl-1H-benzimidazole (hereinafter, referred to as present active compound 206).
WORKUP
后处理
- temperaturecool
- stirringthe mixture was stirred for 1.5 hours at room temperature
- extractionthe mixture was extracted three times with ethyl acetate
- dry with materialThe organic layer was dried over magnesium sulfate
- concentrationconcentrated under reduced pressure