반응 #1824320

ord-4ca98fb0e6f6433e8d78c63ea080cf22

반응 방정식

O=C1CSCCS1
2,5-dithia cyclohexanone
CCCCCCCCCCOC(=O)[C@@H](N)CS.Cl
cysteine decyl ester hydrochloride
CCN(CC)CC
triethyl amine
CCCCCCCCCCOC(=O)C(CS)NC(=O)CSCCS
S-(2-mercaptoethyl)-N-(2-mercapto-1(decyloxycarbonyl)-ethyl)-mercaptoacetamide

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONare added
  2. 2
    세척washed three times with 2% aqueous citric acid, saturated sodium hydrogencarbonate solution
  3. 3
    건조After drying above sodium sulfate
  4. 4
    기타the solvent is evaporated under reduced pressure
  5. 5
    기타The oily residue is crystallized by trituration with diethyl ether

실험 절차

13.42 g (0.1 mol) of 2,5-dithia cyclohexanone dissolved in 250 ml of anhydrous dichloromethane are added by dropping, and in an argon atmosphere, to a solution of 29.79 g (0.1 mol) of cysteine decyl ester hydrochloride and 10.12 g (0.1 mol) of triethyl amine in 500 ml of anhydrous dichloromethane. The reaction mixture is kept agitated overnight at room temperature and then washed three times with 2% aqueous citric acid, saturated sodium hydrogencarbonate solution and with water. After drying above sodium sulfate, the solvent is evaporated under reduced pressure. The oily residue is crystallized by trituration with diethyl ether.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05961954uspto-grants-1999_10