Reaktion #462858

Reaktionsgleichung

2-chloro-5nitrobenzenesulfonyl chloride

dimethylamine hydrochloride

triethylamine

→

title compound

Ausbeute 73.8%

N,N-dimethyl-2-chloro-5-nitrobenzenesulfonamide

Ausbeute 73.8%

Lösungsmittel

methylene chloride

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturto reflux
2. 2
   workup.ADDITIONAfter completion of the addition
3. 3
   Temperaturthe reaction mixture was refluxed for 20 minutes
4. 4
   Einengenconcentrated by rotatory evaporation
5. 5
   workup.ADDITIONThe residue was treated with water
6. 6
   Filtrationthe resulting solid was filtered
7. 7
   Sonstigerecrystallized from ethanol

Vorschrift

To a solution of 80 g of 2-chloro-5nitrobenzenesulfonyl chloride (Example A-1 above) in 200 ml of methylene chloride heated to reflux, was slowly added a solution of 30 g of dimethylamine hydrochloride in 30 ml of water followed by a dropwise addition of triethylamine. After completion of the addition, the reaction mixture was refluxed for 20 minutes, cooled to room temperature and concentrated by rotatory evaporation. The residue was treated with water and the resulting solid was filtered and recrystallized from ethanol, affording 61 g of the title compound, mp 138°-140° C.

Quelle