反応 #2383767

反応方程式

N,N-bis-(tert-butoxycarboxy-methyl)-2-bromoethylamine

diisopropylethylamine

ethylmercaptan

→

N,N-Bis-(tert-butoxycarboxy-methyl)-S-ethyl-2-mercaptoethylamine

溶媒

dichloromethane

反応条件

後処理

1. 1
   温度The reaction mixture is refluxed overnight
2. 2
   抽出Then, the solution is extracted twice with semi-saturated, aqueous sodium bicarbonate solution
3. 3
   その他The organic phase is dried on sodium sulfate
4. 4
   その他the solvent is evaporated in a vacuum
5. 5
   その他The residue is chromatographed on silica gel (eluant: dichloromethane/methanol 99:1)

実験手順

3.52 g (10 mmol) of N,N-bis-(tert-butoxycarboxy-methyl)-2-bromoethylamine is dissolved in 50 ml of absolute dichloromethane and mixed with 1.29 g (10 mmol) of diisopropylethylamine and 0.621 g (10 mmol) of ethylmercaptan. The reaction mixture is refluxed overnight. Then, the solution is extracted twice with semi-saturated, aqueous sodium bicarbonate solution. The organic phase is dried on sodium sulfate, and the solvent is evaporated in a vacuum. The residue is chromatographed on silica gel (eluant: dichloromethane/methanol 99:1).

出典