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 the solution of 11.15 g of 3-hydroxy-3,3-diphenylpropionitrile, 13.4 g of iodo acetaldehyde diethylacetal, and 0.9 g of tetra-n-butylammonium hydrogen sulfate in 40 ml of methylene chloride, 10 ml of 50% aqueous sodium hydroxide are added and the mixture is well stirred at room temperature for 24 hours. It is washed with water, dried and evaporated, to give the 2-(2-cyano-1,1-diphenylethoxy)-acetaldehyde diethylacetal as an oil which is sufficiently pure to be used without purification. The solution of 6.8 g thereof in 100 ml of diethyl ether is added dropwise to the stirred suspension of 1.15 g of lithium aluminum hydride in 20 ml of diethyl ether, while cooling with ice. Upon completion of the addition, the mixture is stirred under reflux for 6 hours. It is cooled and excess hydride is destroyed by successive addition of 1.15 ml of water, 1.15 ml of 15% aqueous sodium hydroxide and 3.45 ml more water. The mixture is filtered, the filtrate is dried and evaporated to give the oily 2-(3-amino-1,1-diphenylpropoxy)-acetaldehyde diethylacetal.
WORKUP
后处理
- washIt is washed with water
- customdried
- customevaporated