Reaktion #935811

Reaktionsgleichung

N-cyclohexylbromomethanesulfonamide

1,1,2,2-tetrachloroethylsulfenyl chloride

→

N-cyclohexyl-N-(1,1,2,2-tetrachloroethylthio)-bromomethanesulfonamide

Lösungsmittel

triethylamine

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONAfter the addition
2. 2
   Temperaturunder reflux for 2 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 5.1 g (0.051 mol) sample of triethylamine was added dropwise to a cooled (20° C.) solution of 11 g (0.043 mol) N-cyclohexylbromomethanesulfonamide and 10.1 g (0.043 mol) 1,1,2,2-tetrachloroethylsulfenyl chloride. After the addition was completed, the reaction was stirred at ambient temperature for 2 hours and then under reflux for 2 hours. The reaction mixture was then cooled, washed with water, dried over magnesium sulfate and evaporated under reduced pressure to give the N-cyclohexyl-N-(1,1,2,2-tetrachloroethylthio)-bromomethanesulfonamide product, which after crystallization from dioxane melted at 38°-40° C. The elemental analysis for the product is tabulated in Table I under Compound No. 8.

Quelle