Hydroxyethyl disulfide → 2-Methanesulfonyloxyethyl disulfide

HRID 1840426

反応式

HRID 1840426 の反応式
C(N(CC)C(C)C)(C)C.[CH3:10][S:11](Cl)(=[O:13])=[O:12].[OH:15][CH2:16][CH2:17][S:18][S:19][CH2:20][CH2:21][OH:22]>ClCCl>[CH3:10][S:11]([O:15][CH2:16][CH2:17][S:18][S:19][CH2:20][CH2:21][O:22][S:11]([CH3:10])(=[O:13])=[O:12])(=[O:13])=[O:12]

参加物

5

反応物 3

HCID 15906Hydroxyethyl disulfideHCID 31297Methanesulfonyl chlorideHCID 81531Diisopropylethylamine

生成物 1

HCID 231172092-Methanesulfonyloxyethyl disulfide

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

N,N-Diisopropylethylamine (4.35 ml) and 1.70 ml of methanesulfonyl chloride were added to a suspension of 1.22 ml of 2-hydroxyethyl disulfide in 30 ml of dichloromethane at −40° C. under an argon atmosphere. The mixture was stirred at that temperature for 30 min. The reaction solution was then diluted with dichloromethane, and the diluted solution was washed with an dilute aqueous hydrochloric acid solution, an aqueous sodium hydrogencarbonate solution, and water in that order, and was dried over anhydrous magnesium sulfate. The solvent was removed by distillation under the reduced pressure to prepare 3.08 g of 2-methanesulfonyloxyethyl disulfide.

後処理

  1. washthe diluted solution was washed with an dilute aqueous hydrochloric acid solution
  2. dry with materialan aqueous sodium hydrogencarbonate solution, and water in that order, and was dried over anhydrous magnesium sulfate
  3. customThe solvent was removed by distillation under the reduced pressure
  4. customto prepare 3.08 g of 2-methanesulfonyloxyethyl disulfide

出典と根拠

ORDレコード
ord-d13d244bb92a4400a4f1dbd341cc93ce
出典データセット
uspto-grants-2004_01
特許番号
US06680313B2

関連ノート

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