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
Lithium aluminum hydride (1.4 g) is suspended in tetrahydrofuran (50 ml) and thereto is added dropwise a 2-(cyclopropylmethyl-propyl-amino)-5-trifluoromethyl-benzaldehyde oxime (5.7 g) in tetrahydrofuran (20 ml) under ice-cooling, and the mixture is stirred at room temperature overnight. To the reaction solution are added water (1.4 ml), a 2N-aqueous sodium hydroxide solution (2.8 ml) and water (2.8 ml) successively under ice-cooling, and the insoluble material is removed by filtration and the filtrate is concentrated under reduced pressure. The resulting residue is purified by NH-silica gel column chromatography (chloroform:ethyl acetate=10:1) to give (2-aminomethyl-4-trifluoromethyl-phenyl)-cyclopropylmethyl-propyl-amine as a crude product (5.1 g).
WORKUP
后处理
- temperaturecooling
- customthe insoluble material is removed by filtration
- concentrationthe filtrate is concentrated under reduced pressure
- customThe resulting residue is purified by NH-silica gel column chromatography (chloroform:ethyl acetate=10:1)