反応 #2383769

反応方程式

S-methyl-thioglycolic acid

N-hydroxysuccinimide

2-methylthio-ethylamine

dicyclohexylcarbodiimide

→

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

溶媒

methylene chloride

methylene chloride

反応条件

後処理

1. 1
   ろ過The precipitate is filtered off
2. 2
   洗浄the filtrate is washed twice with semi-saturated sodium bicarbonate solution and once with water
3. 3
   乾燥dried with sodium sulfate
4. 4
   濃縮concentrated by evaporation
5. 5
   その他The residue is purified by chromatography with the mobile solvent system of methylene chloride/methanol

実験手順

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.

出典