Reaktion #331706
ord-b8fd1201b5654d798122c4747976812a
Reaktionsgleichung
Methanesulphonyl chloride
N,N-dimethyl-1,3-phenylenediamine
sodium hydroxide
→
material
Ausbeute 79.0%
N-[3-(dimethylamino)phenyl]methanesulphonamide
Ausbeute 79.0%
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1ExtraktionThe mixture was extracted with chloroform (3×15 cm3)
- 2TrocknenThe combined extracts were dried over sodium sulphate
- 3Filtrationfiltered
- 4Sonstigethe solvent removed under reduced pressure
Vorschrift
Methanesulphonyl chloride (838 mg, 7.35 mmol) was added slowly to a cooled solution (5° C.) of N,N-dimethyl-1,3-phenylenediamine (1.00 g, 7.35 mmol) and sodium hydroxide (5M, 1.5 cm3) in water (10 cm3). The reaction was allowed to warm to room temperature overnight. The mixture was extracted with chloroform (3×15 cm3). The combined extracts were dried over sodium sulphate, filtered and the solvent removed under reduced pressure. Column chromatography (1:20 methanol/dichloromethane) gave the target material as a brown oil (1.24 g, 79%).