HRID54612

反应详情

EQUATION

反应方程式

HRID 54612 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

tert-Butyl bromoacetate (32.3 ml; 0.2 mol) is slowly added dropwise, while cooling in ice, to a solution of N-benzylethanolamine (30.2 g; 0.2 mol) and triethylamine (27.9 ml; 0.2 mol) in anhydrous N,N-dimethylformamide (200 ml). The mixture is stirred at room temperature for 22 h and is then concentrated in vacuo. The residue is subsequently distilled repeatedly with toluene. The resulting oil is taken up in dichloromethane (400 ml) and extracted twice by shaking with water (160 ml on each occasion). The organic phase is dried (magnesium sulphate) and concentrated. Yield: 47.8 g (90%), colourless oil.

WORKUP

后处理

  1. concentrationis then concentrated in vacuo
  2. distillationThe residue is subsequently distilled repeatedly with toluene
  3. extractionextracted twice
  4. stirringby shaking with water (160 ml on each occasion)
  5. dry with materialThe organic phase is dried (magnesium sulphate)
  6. concentrationconcentrated