Sodium Iodide → HCID 11267746, Verbindung

HRID 2184162

Reaktionsgleichung

Reaktionsgleichung von HRID 2184162
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([S:11](Cl)(=O)=O)[CH:6]=[CH:7][C:8]=1[O:9][CH3:10].[Na+].[I-].FC[C:19]([O:21][C:22](=O)[CH2:23]F)=O>CC(C)=O>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([S:11][S:11][C:5]2[CH:6]=[CH:23][C:22]([O:21][CH3:19])=[C:3]([O:2][CH3:1])[CH:4]=2)[CH:6]=[CH:7][C:8]=1[O:9][CH3:10]

Komponenten

5

Edukt 3

HCID 5238Sodium IodideHCID 67886Acetic acid, 2-fluoro-, 1,1'-anhydrideHCID 27341833,4-Dimethoxybenzenesulfonyl chloride

Produkt 1

HCID 11267746HCID 11267746, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 180AcetoneLösungsmittel

Versuchsvorschrift

3,4-dimethoxyphenylsulfonyl chloride (2.3 mmol) was dissolved in acetone (60 mL), and then NaI (3.4 g, 23 mmol) and fluoroacetic anhydride (1.45 mL, 6.9 mmol) were added and the mixture was stirred at room temperature for one hour. The reaction solution was concentrated, water was added, extraction was performed with ether and the organic layer was further washed with aqueous sodium thiosulfate, water and saturated saline. After drying over magnesium sulfate and vacuum concentration, the residue was purified with a silica gel column (hexane) to obtain 3,4-dimethoxyphenyldisulfide as a light yellow crystalline compound (58% yield). The NMR and mass spectral data for the obtained compound were as follows:

Aufarbeitung

  1. concentrationThe reaction solution was concentrated
  2. additionwater was added
  3. extractionextraction
  4. washthe organic layer was further washed with aqueous sodium thiosulfate, water and saturated saline
  5. dry with materialAfter drying over magnesium sulfate and vacuum concentration
  6. customthe residue was purified with a silica gel column (hexane)

Quellen und Nachweise

ORD-Eintrag
ord-03b07f8954b243fda6cc6cb8b2bc2cb9
Quelldatensatz
uspto-grants-2005_05
Patentnummer
US06900307B1

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