Reaktion #707993

Reaktionsgleichung

methyl methylsulfonylacetate

carbon disulfide

potassium hydroxide

cis-1,2-dichloroethylene

→

title compound

Ausbeute 83.0%

methyl 1,3-dithiol-2-ylidenemethylsulfonylacetate

Ausbeute 83.0%

Lösungsmittel

dimethylformamide

water

chloroform

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONwas added under ice-
2. 2
   Temperaturcooling
3. 3
   workup.ADDITIONwere added
4. 4
   Sonstigethe resulting organic layer was separated
5. 5
   SonstigeUpon removal of the solvent
6. 6
   workup.DISTILLATIONby distillation under reduced pressure

Vorschrift

To a mixture of 15.2 g of methyl methylsulfonylacetate, 7.6 g of carbon disulfide and 200 ml of dimethylformamide, 14.0 g of potassium hydroxide was added under ice-cooling. The resultant mixture was stirred for 3 hours. Thereafter, 9.7 g of cis-1,2-dichloroethylene was added, followed by stirring at 80° C. for 4 hours. After cooling the reaction mixture, chloroform and water were added and the resulting organic layer was separated. Upon removal of the solvent by distillation under reduced pressure, 20.9 g of the title compound was obtained as pale yellow crystals. Upon recrystallization from a mixed solvent of chloroform and n-hexane, they turned to white crystals. Melting point: 166°-168° C. (decomposed).

Quelle