反应详情

To a mixture of 2-amino-4-chlorobenzoic acid (4.5 g, 26.23 mmol) and cyclohexanone (2.72 mL, 26.23 mmoL) was added 22 mL phosphorus oxychloride. The mixture was heated to reflux for 3 hours. The excess phosphorus oxychloride was distilled off and the resulting mixture was treated with saturated sodium bicarbonate. The light brown precipitate was filtered, rinsed with water and dried under vacuum to give the desired product 6.50 g (25.77 mmoL, 98.2%).

1. temperatureThe mixture was heated
2. temperatureto reflux for 3 hours
3. distillationThe excess phosphorus oxychloride was distilled off
4. additionthe resulting mixture was treated with saturated sodium bicarbonate
5. filtrationThe light brown precipitate was filtered
6. washrinsed with water
7. customdried under vacuum