HRID888758

反应详情

EQUATION

反应方程式

HRID 888758 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. additionAdded dropwise to this suspension
  2. temperatureThe mixture is subsequently heated
  3. temperatureat reflux for 2.5 hours
  4. temperatureAfter cooling
  5. filtrationThe mixture is then filtered
  6. dry with materialthe filtrate is dried over calcium chloride
  7. concentrationconcentrated
  8. customThe orange oil obtained
  9. distillationis subsequently distilled under reduced pressure (overhead temperature=46° C., p=0.016 mbar)