Triethylamine → HCID 12984268、化合物

HRID 1737138ノート

反応式

HRID 1737138 の反応式
[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]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 5427241,4-Dithian-2-oneHCID 86754565HCID 86754565、化合物

生成物 1

HCID 12984268HCID 12984268、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-4ca98fb0e6f6433e8d78c63ea080cf22
出典データセット
uspto-grants-1999_10
特許番号
US05961954

反応ノート

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