反应详情

To a solution of 2-((4-chlorophenyl)carbonylamino)-4,5-dimethoxybenzamide (1.0 g, 2.99 mmol) in ethanol (10 mL) was added aqueous NaOH solution (15 mL) at rt for 10 min. The reaction mixture was refluxed for 10 min and allowed to rt. The mixture was poured into ice cold water and stirred for 10 min EtOAc (20 mL) was added to the solution and stirred for 5 min. The separated solid was filtered, washed with ice cold water and dried to the product as a white color solid (900 mg, 95%), mp>360° C. 1H NMR (400 MHz, DMSO-d6): δ 12.47 (1H, s), 8.19 (2H, d, J=8.6 Hz), 7.62 (2H, d, J=8.6 Hz), 7.50 (1H, s), 7.23 (1H, s), 3.94 (3H, s), 3.90 (3H, s); LC-MS (positive ion mode): m/z 317, 319 (M+H)±.

1. temperatureThe reaction mixture was refluxed for 10 min
2. customallowed to rt
3. additionThe mixture was poured into ice cold water
4. additionwas added to the solution
5. filtrationThe separated solid was filtered
6. washwashed with ice cold water
7. dry with materialdried to the product as a white color solid (900 mg, 95%), mp>360° C