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
- 35 °C
PROCEDURE
实验过程
In a 1.5 liter sulfonating flask, 10.7 g (0.282 mol) of lithium aluminium hydride are suspended in 620 ml of diethyl ether. Then 55.9 g (0.282 mol) of 3-(3-[1,3]dioxolan-2-yl-propylamino)butyronitrile in solution in 210 ml of diethyl ether are slowly added dropwise. The mixture is subsequently heated at 35° C. for three hours. After cooling to 0° C., 10.7 g of water, 10.7 g of 10% strength NaOH and then a further 32.1 g of water are carefully added dropwise. The reaction solution is filtered over Hyflo and concentrated under reduced pressure. This gives 49.86 g of 3-{3-([1,3]dioxolan-2-yl)propylamino}-1-aminobutane as a reddish liquid which is used without further purification in the next stage.
WORKUP
后处理
- temperatureAfter cooling to 0° C.
- filtrationThe reaction solution is filtered over Hyflo
- concentrationconcentrated under reduced pressure
- customThis gives 49.86 g of 3-{3-([1,3]dioxolan-2-yl)propylamino}-1-aminobutane as a reddish liquid which is used without further purification in the next stage