Water → N'-hydroxy-6-[4-methoxy-3-(3,3,6,6-tetramethyl-1,8-dioxo-2,3,4,5,6,7,8,9-octahydro-1H-xanthen-9-yl)phenyl]pyridine-2-carboximidamide

Participants

Reaction Steps

Sodium carbonate (122 mg, 1.15 mmol) was added to a suspension of the 6-[4-methoxy-3-(3,3,6,6-tetramethyl-1,8-dioxo-2,3,4,5,6,7,8,9-octahydro-1H-xanthen-9-yl)phenyl]pyridine-2-carbonitrile produced in Example 6 (410 mg, 0.85 mmol) and hydroxylamine hydrochloride (73.8 mg, 1.06 mmol) in methanol (8.2 ml) at room temperature, and the mixture thus obtained was then stirred at the same temperature as above for 25 hours. Thereafter, water was added to the reaction solution, and the mixed solution was then extracted with dichloromethane. The organic layer thus obtained was dried over anhydrous sodium sulfate. The solvent was distilled away under reduced pressure to obtain the title compound (429 mg, yield: 98%).

Provenance & Evidence