Hydroxyethyl disulfide → 2-Methanesulfonyloxyethyl disulfide

HRID 1840426

Reaktionsgleichung

Reaktionsgleichung von HRID 1840426
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]

Komponenten

5

Edukt 3

HCID 15906Hydroxyethyl disulfideHCID 31297Methanesulfonyl chlorideHCID 81531Diisopropylethylamine

Produkt 1

HCID 231172092-Methanesulfonyloxyethyl disulfide

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel2×

Versuchsvorschrift

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.

Aufarbeitung

  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

Quellen und Nachweise

ORD-Eintrag
ord-d13d244bb92a4400a4f1dbd341cc93ce
Quelldatensatz
uspto-grants-2004_01
Patentnummer
US06680313B2

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