Hydroxyamine hydrochloride → HCID 430947, compound

Participants

Reaction Steps

In ethanol (10 ml) was dissolved metal sodium (0.4 g) and thereto was further added hydroxylamine hydrochloride (0.8 g). To the solution was added a solution of 1,2-benzisoxazole-3-acetohydroximic chloride (5.0 g) in ethanol (40 ml) under ice-cooling and the mixture was stirred for hour. The mixture was distilled under a reduced pressure to remove the solvent. To the residue was added chloroform and the insoluble substance was filtered off, and the filtrate was subjected to silica gel column chromatography and eluted with 5 % methanol-chloroform. The resulting precipitated crystallines were separated by filtration and recrystallized from ethanol to give the desired compound (1.0 g). m.p. 161° to 163°C.

Provenance & Evidence