Reaktion #697938

Reaktionsgleichung

Water

methanethiol

ethyl 3-chloro-2-(N-ethyl-N-methylsulphonylamino)-4-fluorobenzoate

potassium carbonate

→

ethyl 3-chloro-2-(N-ethyl-N-methylsulphonylamino)-4-(methylthio)benzoate

Lösungsmittel

DMF

DMF

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturwarmed to ambient temperature over 2.5 hours
2. 2
   Extraktionthe mixture extracted with ether
3. 3
   Waschenwashed with brine solution
4. 4
   Trocknenwater, dried (anhydrous magnesium sulphate)
5. 5
   Sonstigethe solvent evaporated

Vorschrift

A solution of methanethiol (4 ml) in dry DMF was added to a mixture of ethyl 3-chloro-2-(N-ethyl-N-methylsulphonylamino)-4-fluorobenzoate (7.4 g) and anhydrous potassium carbonate (4.71 g) in DMF at -40° C. The mixture was maintained at -10° C. for 1 hour, then warmed to ambient temperature over 2.5 hours. Water was added and the mixture extracted with ether, washed with brine solution then water, dried (anhydrous magnesium sulphate) and the solvent evaporated to give ethyl 3-chloro-2-(N-ethyl-N-methylsulphonylamino)-4-(methylthio)benzoate (8.3 g) as a white powder, m.p. 109-110.5° C.

Quelle