Реакция #2383769
ord-28b7090dc04a4b5398f0f5ee3b6792e1
Уравнение реакции
S-methyl-thioglycolic acid
N-hydroxysuccinimide
2-methylthio-ethylamine
dicyclohexylcarbodiimide
→
S-methyl-thioglycolic Acid-N-(2-methylthioethyl)-amide
Реактанты
Реагенты
Нет
Растворители
Условия реакции
Подробные условия
See reaction.notes.procedure_details.
Обработка
- 1ФильтрацияThe precipitate is filtered off
- 2Промывкаthe filtrate is washed twice with semi-saturated sodium bicarbonate solution and once with water
- 3Сушкаdried with sodium sulfate
- 4Концентрированиеconcentrated by evaporation
- 5ДругоеThe residue is purified by chromatography with the mobile solvent system of methylene chloride/methanol
Методика
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.