Ammonium Persulfate → (3,5-Dimethyl-4-nitropyridin-2-yl)methanol

Beteiligte Stoffe

Reaktionsschritte

3,5-Dimethyl-4-nitropyridine-N-Oxide-dimethyl sulfate adduct (VI) (220 gm, 0.75 mole) was dissolved in methanol (1.0 ltr) and the solution heated to reflux. A solution of ammonium persulfate (140 gm) in water (200 ml) was added dropwise over 4 hours after which reflux was continued for 4 hours. Methanol was distilled off under reduced pressure and the residue was basified to pH 10 by addition of caustic lye (105 ml). The mixture was extracted with dichloromethane (2×400 ml). The dichloromethane layer was dried over sodium sulfate and filtered. The product was used as its solution in dichloromethane for the next reaction.

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