Reaktion #465495

Reaktionsgleichung

4-amino-N-(2-chloro-6-trifluoromethyl-pyridin-4-yl)-benzenesulfonamide

methylamine

N-[4-(2-chloro-6-trifluoromethyl-pyridin-4-ylsulfamoyl)-phenyl]-acetamide

→

4-amino-N-(2-methylamino-6-trifluoromethyl-pyridin-4-yl)-benzenesulfonamide

Ausbeute 70.0%

Lösungsmittel

methylamine

ethanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeto evaporate
2. 2
   workup.DISSOLUTIONthe residue was dissolved in ethanol
3. 3
   workup.ADDITIONtreated with 2 g of silica gel
4. 4
   Einengenconcentrated
5. 5
   Sonstigethe residue was chromatographed on silica gel with ethyl acetate/hexane 1:2

Vorschrift

0.052 g (0.00015 mol) of 4-amino-N-(2-chloro-6-trifluoromethyl-pyridin-4-yl)-benzenesulfonamide was stirred in 30 ml of 8M methylamine in ethanol in an autoclave at 135° C. for 80 hours. The methylamine was allowed to evaporate, the residue was dissolved in ethanol, treated with 2 g of silica gel, concentrated and the residue was chromatographed on silica gel with ethyl acetate/hexane 1:2. There was obtained 0.036 g (70%) of 4-amino-N-(2-methylamino-6-trifluoromethyl-pyridin-4-yl)-benzenesulfonamide as colorless crystals; m.p.: >68° C. (dec.).

Quelle