반응 #2383769

반응 방정식

S-methyl-thioglycolic acid

N-hydroxysuccinimide

2-methylthio-ethylamine

dicyclohexylcarbodiimide

→

S-methyl-thioglycolic Acid-N-(2-methylthioethyl)-amide

용매

methylene chloride

methylene chloride

반응 조건

후처리

1. 1
   여과The precipitate is filtered off
2. 2
   세척the filtrate is washed twice with semi-saturated sodium bicarbonate solution and once with water
3. 3
   건조dried 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

6 ml of 2-methylthio-ethylamine is dissolved in 250 ml of methylene chloride, mixed with 6.84 g of S-methyl-thioglycolic acid and with 7.42 g of N-hydroxysuccinimide and mixed drop by drop with 13.3 g of dicyclohexylcarbodiimide in 250 ml of methylene chloride under a cover-gas atmosphere. It is stirred, for 3 more hours at room temperature. The precipitate is filtered off, the filtrate is washed twice with semi-saturated sodium bicarbonate solution and once with water, dried with sodium sulfate and concentrated by evaporation. The residue is purified by chromatography with the mobile solvent system of methylene chloride/methanol: Yield 10 g=86.7% of theory.

출처