反应详情

温度

2.5 °C

6.60 g (0.030 mols) of 5-cyano-10,11-dihydro-5H-dibenz[b,f]-azepine (I) are stirred at 50° C. with 50 ml of CCl4. The fluid suspension is added under stirring with 5.6 g (0.0315 mols) of N-bromosuccinimide of purity above 98%, then with 0.37 g (0.0015 mols) of dibenzoylperoxide. Temperature is raised to mild reflux and the mixture is stirred for a further 55 minutes controlling the formed foam, then cooled and solvent is evaporated off. The residue is suspended in toluene (15 ml) at 80° C. for 20 minutes, filtered, the solution is cooled at 0-5° C. for 1 hour, to obtain 8.2 g (83%) of 5-cyano-10-bromo-10,11-dihydro-5H-dibenz[b,f]azepine (II), m.p. 132-9 (with decomposition).

1. additionThe fluid suspension is added
2. temperatureTemperature is raised
3. temperatureto mild reflux
4. temperaturecooled
5. customsolvent is evaporated off
6. waitThe residue is suspended in toluene (15 ml) at 80° C. for 20 minutes
7. filtrationfiltered