反应 #2314310

ord-5ce367e933884c81ae98f7342263b714

反应方程式

c1ccc2c(c1)Nc1ccccc1-c1ccccc1-2
9H-tribenz[b,d,f]azepine
Brc1ccc(Br)cc1
1,4-dibromobenzene
[K+].[OH-]
potassium hydroxide
Brc1ccc(N2c3ccccc3-c3ccccc3-c3ccccc32)cc1
9-(4-bromophenyl)-9H-tribenz[b,d,f]azepine
收率 25.1%

溶剂

反应条件

温度
200°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他the resulting crude product was purified by silica gel column chromatography

实验过程

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 worked up in the same manner as in Example 1, and the resulting crude product was purified by silica gel column chromatography to give 3.8 g (25%) of 9-(4-bromophenyl)-9H-tribenz[b,d,f]azepine.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US06413657B1uspto-grants-2002_07