反应详情

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.

1. filtrationThe precipitate is filtered off
2. washthe filtrate is washed twice with semi-saturated sodium bicarbonate solution and once with water
3. dry with materialdried with sodium sulfate
4. concentrationconcentrated by evaporation
5. customThe residue is purified by chromatography with the mobile solvent system of methylene chloride/methanol