HRID604011
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
2-Fluoro-5-trifluoromethyl-benzaldehyde (1.3 g) and cyclopropylmethyl-propyl-amine (1.15 g) are dissolved in toluene (13 ml), and thereto is added potassium carbonate (2.81 g) and the mixture is stirred at 120° C. overnight. The reaction solution is cooled to room temperature, and thereto are added ethyl acetate and water, and the mixture is separated, and the organic layer is washed with a saturated brine, dried over magnesium sulfate, and concentrated under reduced pressure. The resulting residue is purified by silica gel column chromatography (hexane:ethyl acetate=1:0→97:3) to give 2-(cyclopropylmethyl-propyl-amino)-5-trifluoromethyl-benzaldehyde (1.7 g). MS (m/z): 286 [M+H]+
WORKUP
后处理
- temperatureThe reaction solution is cooled to room temperature
- customthe mixture is separated
- washthe organic layer is washed with a saturated brine
- dry with materialdried over magnesium sulfate
- concentrationconcentrated under reduced pressure
- customThe resulting residue is purified by silica gel column chromatography (hexane:ethyl acetate=1:0→97:3)