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 (Na2SO4) 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. dry with materialThe filtrate is dried (Na2SO4)
6. customthe solvent removed
7. customto give a solid
8. customThe solid (1.1 g) is chromatographed on thick layer silica gel plates