Triethylamine → HCID 12984268, 화합물

HRID 1737138노트

반응식

HRID 1737138 반응식
[C:1]1(=[O:7])[CH2:6][S:5][CH2:4][CH2:3][S:2]1.Cl.[CH2:9]([O:19][C:20](=[O:25])[C@H:21]([CH2:23][SH:24])[NH2:22])[CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH3:18].C(N(CC)CC)C>ClCCl>[SH:2][CH2:3][CH2:4][S:5][CH2:6][C:1]([NH:22][CH:21]([C:20]([O:19][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH3:18])=[O:25])[CH2:23][SH:24])=[O:7]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 5427241,4-Dithian-2-oneHCID 86754565HCID 86754565, 화합물

생성물 1

HCID 12984268HCID 12984268, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

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.

후처리

  1. additionare added
  2. washwashed three times with 2% aqueous citric acid, saturated sodium hydrogencarbonate solution
  3. dry with materialAfter drying above sodium sulfate
  4. customthe solvent is evaporated under reduced pressure
  5. customThe oily residue is crystallized by trituration with diethyl ether

출처 및 근거

ORD 기록
ord-4ca98fb0e6f6433e8d78c63ea080cf22
출처 데이터셋
uspto-grants-1999_10
특허 번호
US05961954

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