반응 #2383771

반응 방정식

methylene chloride

diisopropylethylamine

bis-(2-methylthioethyl)-amine

bromoacetic acid methyl ester

→

N,N-bis-(2-methylthioethyl)-glycine methyl ester

용매

acetonitrile

acetonitrile

acetonitrile

반응 조건

후처리

1. 1
   workup.ADDITIONis added in drops under a cover-gas atmosphere
2. 2
   세척washed twice with saturated sodium bicarbonate solution
3. 3
   건조The organic phase is dried with sodium sulfate
4. 4
   농축concentrated by evaporation
5. 5
   기타the residue is purified by chromatography with the mobile solvent system of methylene chloride/methanol

실험 절차

165 mg of bis-(2-methylthioethyl)-amine (Example 8b) is dissolved in 20 ml of acetonitrile and mixed with 174 μl of diisopropylethylamine. 92.7 μl of bromoacetic acid methyl ester, dissolved in 20 ml of acetonitrile, is added in drops under a cover-gas atmosphere, and the batch is stirred for 18 hours at room temperature. The acetonitrile is drawn off, the residue is taken up with methylene chloride and washed twice with saturated sodium bicarbonate solution. The organic phase is dried with sodium sulfate and concentrated by evaporation, and the residue is purified by chromatography with the mobile solvent system of methylene chloride/methanol: Yield 183 mg=77% of theory.

출처