Phosphorus oxychloride → HCID 58058403, compound

Participants

Reaction Conditions

Reaction Steps

To a solution of 2-bromo-N-(2-(phenylamino)phenyl)benzamide (10.7 g, 29 mmol) in anhydrous 1,4-dioxane (˜100 mL), was added POCl3 (6.92 g, 45 mmol) slowly. The whole was heated to about 100° C. under argon overnight. After cooling the mixture to room temperature, the mixture was poured into ice (˜150 g), and then neutralized with NaHCO3. After filtration, the solid was collected then dissolved in dichloromethane (˜250 mL), which was washed with water (˜250 mL). The aqueous solution was extracted with dichloromethane (˜100 mL×2). The organic phase was combined and dried over Na2SO4, concentrated, and recrystallized in dichloromethane/hexanes to give a light grey solid (6.68 g, 66% yield).

Provenance & Evidence