Dimethyl Sulfoxide → 4-Methyl-1,2-dithiolane-4-carboxylic acid

HRID 41810Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 41810
Cl[CH:2](Cl)[C:3]([CH3:8])(C)[C:4]([OH:6])=[O:5].C([O-])([O-])=O.[Na+].[Na+].C([O-])(=[S:18])C.[K+].C[S:22]([CH3:24])=O>O>[CH3:8][C:3]1([C:4]([OH:6])=[O:5])[CH2:24][S:22][S:18][CH2:2]1

Komponenten

6

Edukt 4

HCID 679Dimethyl SulfoxideHCID 10340Sodium Carbonate2×HCID 103039Propanoic acid, 3,3-dichloro-2,2-dimethyl-HCID 23670855Potassium ethanethioate

Produkt 1

HCID 200693114-Methyl-1,2-dithiolane-4-carboxylic acid

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

8 g of dichloropivalic acid are placed in a 250 ml three-necked flask on which is mounted a condenser and a dropping funnel. The acid is dissolved in 80 ml of water, slowly adding 4.6 g of Na2CO3. A solution of 10.7 g of potassium thioacetate is added dropwise and the reaction medium is brought to reflux. 14.9 g of Na2CO3 are added and the medium is again heated at reflux. After disappearance of the starting material, 7.3 ml of DMSO are added, followed by refluxing. The dithiolane is obtained after acidification by precipitation and drying of the solid under vacuum. A pale yellow solid is obtained.

Aufarbeitung

  1. temperatureto reflux
  2. temperaturethe medium is again heated
  3. temperatureat reflux
  4. temperatureby refluxing

Quellen und Nachweise

ORD-Eintrag
ord-bb176405ee3c4692be973994088b8f98
Quelldatensatz
uspto-grants-2013_09
Patentnummer
US08535647B2

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