Reaktion #935580

Reaktionsgleichung

N-isopropyl chloromethanesulfonamide

1,1,2,2-tetrachloroethylsulfenyl chloride

→

N-isopropyl-N-(trichlorovinylthio)-chloromethanesulfonamide

Lösungsmittel

triethylamine

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONAfter the addition
2. 2
   Temperaturunder reflux for 3 hours
3. 3
   TemperaturThe reaction mixture was then cooled
4. 4
   Waschenwashed with water
5. 5
   Trocknendried over magnesium sulfate
6. 6
   Sonstigeevaporated under reduced pressure

Vorschrift

A 32.3 g (0.32 mol) sample of triethylamine was added dropwise to a cooled (0° C.) solution of 50 g (0.29 mol) N-isopropyl chloromethanesulfonamide and 70 g (0.29 mol) 1,1,2,2-tetrachloroethylsulfenyl chloride. After the addition was completed, the reaction was stirred at ambient temperature for 30 minutes and then under reflux for 3 hours. The reaction mixture was then cooled, washed with water, dried over magnesium sulfate and evaporated under reduced pressure to give the N-isopropyl-N-(trichlorovinylthio)-chloromethanesulfonamide product, which after crystallization from pet. ether melted at 71°-73° C. The product is reported as Compound 1.

Quelle