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
- 0 °C
PROCEDURE
实验过程
A solution (5 mL) of 1-methyl-1H-benzimidazole-6-carbohydrazide (0.20 g, 1.05 mmol), triethylamine (0.18 mL, 1.26 mmol) and carbon disulfide (0.16 mL, 2.63 mmol) in ethanol was heated under reflux overnight. The reaction mixture was cooled to 0° C., potassium hydroxide (58.9 mg, 1.05 mmol) and 3-(trifluoromethyl)benzyl chloride were added, and the resulting mixture was stirred overnight at room temperature. The reaction mixture was diluted with ethyl acetate, washed with water and saturated brine, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (hexane/ethyl acetate=1/3) to give the title compound (49.9 mg, yield 12%) as colorless crystals.
WORKUP
后处理
- temperatureunder reflux overnight
- washwashed with water and saturated brine
- dry with materialdried over anhydrous magnesium sulfate
- concentrationconcentrated under reduced pressure
- customThe residue was purified by silica gel column chromatography (hexane/ethyl acetate=1/3)