反应详情

温度

200 °C

A mixture of 9.2 g (38 mmol) of 9H-tribenz[b,d,f]azepine (synthesized in accordance with J. Org. Chem., vol. 56, p. 3906 (1991)), 44.8 g (190 mmol) of 1,4-dibromobenzene, 5.6 g (100 mmol) of potassium hydroxide, 1.6 g (25 mmol) of copper powder, and 50 ml of decalin was heated at an external temperature of 200° C. for 36 hours in a nitrogen stream while stirring. The reaction mixture was cooled nearly to room temperature, chloroform was added thereto, followed by filtration using Celite to remove the insoluble matter. The filtrate was concentrated. To remove decalin, n-hexane was added to the residue, followed by filtration. The filter cake was purified by silica gel column chromatography to give 3.8 g (25%) of 9-(4-bromophenyl)-9H-tribenz[b,d,f]azepine.

1. temperatureThe reaction mixture was cooled nearly to room temperature
2. filtrationfollowed by filtration
3. customto remove the insoluble matter
4. concentrationThe filtrate was concentrated
5. customTo remove decalin, n-hexane
6. additionwas added to the residue
7. filtrationfollowed by filtration
8. customThe filter cake was purified by silica gel column chromatography