Sodium Chloride → Pyridine, 2,3-dimethyl-, 1-oxide

Participants

Reaction Conditions

Reaction Steps

46.2 g of magnesium monoperoxyphthalate hexahydrate in 150 ml of water were slowly added at room temperature to a solution of 11.32 ml (0.100 mole) of 2,3-dimethylpyridine and 11.2 g of potassium carbonate in 50 ml of water. The reaction was carried out at a pH of 6.5-7.0, adjusted by a solution of potassium carbonate, and the reaction mixture was stirred for three hours at a temperature of from 25 to 30° C. At the end of the reaction, the pH was adjusted to 7.5-8.0, 40 g of sodium chloride were added and the 2,3-dimethylpyridine N-oxide was extracted with methylene chloride. The extraction was repeated from saturated reaction solution. The combined organic phases were dried with sodium sulphate and concentrated to a volume of 60 ml. The yield was 97-98%, determined by HPLC.

Provenance & Evidence