HRID888758
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
50.1 g (1.32 mol) of lithium aluminium hydride are suspended in 500 ml of ether. Added dropwise to this suspension is a solution of 111.9 g (0.88 mol) of 3-[1,3]-dioxolan-2-yl-propionitrile. The mixture is subsequently heated at reflux for 2.5 hours. After cooling, 50 g of water, 50 g of 10% strength sodium hydroxide solution and a further 150 g of water are added. The mixture is then filtered and the filtrate is dried over calcium chloride and concentrated. The orange oil obtained is subsequently distilled under reduced pressure (overhead temperature=46° C., p=0.016 mbar). This gives 68.4 g of 3-[1,3]-dioxolan-2-yl-propylamine.
WORKUP
后处理
- additionAdded dropwise to this suspension
- temperatureThe mixture is subsequently heated
- temperatureat reflux for 2.5 hours
- temperatureAfter cooling
- filtrationThe mixture is then filtered
- dry with materialthe filtrate is dried over calcium chloride
- concentrationconcentrated
- customThe orange oil obtained
- distillationis subsequently distilled under reduced pressure (overhead temperature=46° C., p=0.016 mbar)