Hydrochloric Acid → HCID 67358973, compound

Participants

Reaction Conditions

Reaction Steps

A 1 L three-necked flask was charged with 67.7 g (0.158 mol) N-[2-(4-oxo-4H-3,1-benzoxazin-2-yl)phenyl]-2-naphthalenesulfonamide) and 200 g ethanol. Under stirring, 0.33 g sodium hydroxide (0.0083 mol, correlates to 5.2% of applied raw material) was added. After 15 minutes, the reaction mixture was heated until reflux for 5 hours. Completion of the reaction was monitored by thin layer chromatography. After the 5 hours, the intermediate mixture was cooled to 20° C., and within 20 minutes 4.5 g of 10% hydrochloric acid solution (0.012 mol) was added drop wise. The precipitate consisted of tiny white crystals, and was stirred for 1 hour at room temperature, then filtered by suction, washed with first 150 ml ethanol, then 300 ml water and dried at 85° C. in a circulating air oven.

Provenance & Evidence