Hydroxyamine hydrochloride → 5-p-Methoxybenzyloxy-1-hydroxy-2-hydroxymethyl-4-pyridone

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Reaction Steps

39.3 g of 5-p-methoxybenzyloxy-2-hydroxymethyl-4-pyrone is dissolved in 600 ml of pyridine, then 52.2 g of hydroxylamine hydrochloride is added thereto, and reacted at 70°-75° C. for 2.5 hours. After the reaction, the reaction mixture is concentrated to about 100 ml and, after adding 100 ml of water thereto, added to a mixed solution of 75 ml of hydrochloric acid and 225 ml of water with ice cooling. The pH is adjusted to 2-2.5, and stirring is conducted at the same temperature for 30 minutes. The formed crystals are filtered off, washed with water and then dried to obtain 16.6 f of the title compound.

Provenance & Evidence