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
10.0 g (51.0 mmol) 2-bromophenylacetonitrile were dissolved in 80 ml ether and the solution was added dropwise to 5.81 g (153 mol) lithium aluminium hydride in 230 ml ether. The mixture was heated under reflux for three hours, while stirring, and, after cooling, 80 ml potassium hydroxide solution (10 wt. %) were slowly added dropwise, with vigorous stirring. After stirring overnight, the supernatant was decanted off, the residue was rinsed twice with 100 ml ether each time, the combined organic phases were dried over anhydrous magnesium sulfate and filtered and the filtrate was concentrated on a rotary evaporator (500-10 mbar). 9.48 g 2-(2-bromo-phenyl)-ethylamine (93% of theory) were obtained in this manner.
WORKUP
后处理
- temperatureThe mixture was heated
- temperatureunder reflux for three hours
- temperatureafter cooling
- stirringAfter stirring overnight
- customthe supernatant was decanted off
- washthe residue was rinsed twice with 100 ml ether each time
- dry with materialthe combined organic phases were dried over anhydrous magnesium sulfate
- filtrationfiltered
- concentrationthe filtrate was concentrated on a rotary evaporator (500-10 mbar)