Triethylamine → HCID 430947, compound

Participants

Reaction Steps

To a solution of 1,2-benzisoxazole-3-acetohydroximic chloride (0.4 g) in chloroform (80 ml) was added a solution of triethylamine (3.2 g) in chloroform (40 ml) under ice-cooling and the mixture was stirred for 4 hours under ice-cooling. The mixture was distilled under a reduced pressure to remove the solvent. To the residue was added benzene and the precipitate of triethylamine hydrochloride was filtered off. To the filtrate was passed through ammonia gas under ice-cooling for a period of 1 hour and further at reflux temperature for 3 hours. The mixture was distilled under a reduced pressure to remove the solvent and the residue was subjected to silica gel column chromatography and eluted with 5 % methanol-chloroform. The resulting crystallines were recrystallized from ethanol to give the desired compound (0.1 g). m.p. 160° to 162°C.

Provenance & Evidence