反応 #82890

反応方程式

tert-Butyl bromoacetate

N-benzylethanolamine

triethylamine

→

N-Benzyl-N-(2-hydroxyethyl)-glycine tert-butyl ester

溶媒

N,N-dimethylformamide

反応条件

後処理

1. 1
   濃縮is then concentrated in vacuo
2. 2
   workup.DISTILLATIONThe residue is subsequently distilled repeatedly with toluene
3. 3
   抽出extracted twice
4. 4
   workup.STIRRINGby shaking with water (160 ml on each occasion)
5. 5
   乾燥The organic phase is dried (magnesium sulphate)
6. 6
   濃縮concentrated

実験手順

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.

出典