Hydroxyamine hydrochloride → N-[(2,3-Difluoro-6-methoxyphenyl)methylidene]hydroxylamine

Participants

Reaction Steps

At 20-25° C., a solution of 29.4 g of 2-methoxy-5,6-difluoro-benzaldehyde (according to Ex. 27 of WO 97/03071) was added dropwise with stirring to a mixture of 16.0 g of hydroxylamine hydrochloride, 18.9 g of sodium acetate and 110 ml of 90% strength aqueous methanol. The mixture was stirred for 16 hours, the methanol was evaporated, the mixture was made into a paste using 250 ml of water and then washed and dried, giving 28.3 g of the desired product of m.p. 199-201° C.

Provenance & Evidence