反应详情

2-Methoxybenzoyl chloride (10.2 mL, 75.81 mmol) was added to a mixture of anthranilonitrile (7.46 g, 63.18 mmol) and potassium carbonate (43.76 g, 315.90 mmol) in diethyl ether (400 mL) at reflux. After 24 hours the solution was cooled and water (60 mL) was added. The resulting white solid was collected and washed with water (20 mL) and diethyl ether (50 mL). The solid was suspended in a mixture of 16% w/v aqueous sodium hydroxide (200 mL) and hydrogen peroxide (50 mL of a 30% v/v aqueous solution) and refluxed for 20 hours. The resulting pale yellow solution was cooled and acidified with acetic acid. The resulting precipitate was collected and washed with water to give the title compound as a white solid (4.94 g, 33%).

1. temperatureat reflux
2. temperatureAfter 24 hours the solution was cooled
3. customThe resulting white solid was collected
4. washwashed with water (20 mL) and diethyl ether (50 mL)
5. additionThe solid was suspended in a mixture of 16%
6. temperaturerefluxed for 20 hours
7. temperatureThe resulting pale yellow solution was cooled
8. customThe resulting precipitate was collected
9. washwashed with water