تفاعل #2383769

ord-28b7090dc04a4b5398f0f5ee3b6792e1

معادلة التفاعل

CSCC(=O)O
S-methyl-thioglycolic acid
O=C1CCC(=O)N1O
N-hydroxysuccinimide
CSCCN
2-methylthio-ethylamine
C(=NC1CCCCC1)=NC1CCCCC1
dicyclohexylcarbodiimide
CSCCNC(=O)CSC
S-methyl-thioglycolic Acid-N-(2-methylthioethyl)-amide

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    ترشيحThe precipitate is filtered off
  2. 2
    غسيلthe filtrate is washed twice with semi-saturated sodium bicarbonate solution and once with water
  3. 3
    تجفيفdried with sodium sulfate
  4. 4
    تركيزconcentrated by evaporation
  5. 5
    أخرىThe residue is purified by chromatography with the mobile solvent system of methylene chloride/methanol

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US06488909B1uspto-grants-2002_12