反应详情

温度

80 °C

To a mixture of 1.37 g (5 mmol) of 4-[(2-methylbenzoyl)amino]benzoyl chloride and 0.061 g of 4-(dimethylamino)pyridine in 4 ml of pyridine is added 0.975 g (5 mmol) of 10,11-dihydro-5H-dibenz[b,f]azepine. The mixture is heated at 80° C. for 18 hours and then 0.2 g of sodium hydride (60% in oil) (5 mmol) is added. The mixture is refluxed for 2 hours, diluted with dichloromethane and water and then filtered. To the filtrate is added 1N HCl and the mixture filtered. The filtrate is dried (Na2 SO4) and the solvent removed to give a solid. The solid (1.1 g) is chromatographed on thick layer silica gel plates to give 70 mg of yellow solid, m.p. 112°-118° C.

1. temperatureThe mixture is refluxed for 2 hours
2. filtrationfiltered
3. additionTo the filtrate is added 1N HCl
4. filtrationthe mixture filtered
5. customThe filtrate is dried (Na2 SO4)
6. customthe solvent removed
7. customto give a solid
8. customThe solid (1.1 g) is chromatographed on thick layer silica gel plates