Hydroxyethyl disulfide → 2-Methanesulfonyloxyethyl disulfide

HRID 1840426

반응식

HRID 1840426 반응식
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]

참가 물질

5

반응물 3

HCID 15906Hydroxyethyl disulfideHCID 31297Methanesulfonyl chlorideHCID 81531Diisopropylethylamine

생성물 1

HCID 231172092-Methanesulfonyloxyethyl disulfide

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-d13d244bb92a4400a4f1dbd341cc93ce
출처 데이터셋
uspto-grants-2004_01
특허 번호
US06680313B2

연결된 노트

불러오는 중…