反应详情

(Biphenyl-4-yl)-phenylamine (35.0 g) and DMF (700 ml) were added and dissolved in a nitrogen-substituted reaction vessel, and N-bromosuccinimide (8.5 g) was added under ice-cooled conditions. The reaction temperature was raised to room temperature while adding N-bromosuccinimide (17.0 g) in two separate portions. After being stirred for 25.5 hours, the reaction solution was dropped to water (3,500 ml), and the precipitated solid was collected by filtration. Toluene (2,500 ml) was added to dissolve the solid, and the solid was dried over magnesium sulfate. After filtration, the filtrate was concentrated. The resulting concentrate was dispersed and washed by addition of n-hexane (500 ml), and dried overnight under reduced pressure to obtain a reddish solid of (biphenyl-4-yl)-(4-bromophenyl)amine (44.1 g; yield 95.4%).

1. additionwas added under ice-
2. temperaturecooled conditions
3. customseparate portions
4. additionthe reaction solution was dropped to water (3,500 ml)
5. filtrationthe precipitated solid was collected by filtration
6. additionToluene (2,500 ml) was added
7. dissolutionto dissolve the solid
8. dry with materialthe solid was dried over magnesium sulfate
9. filtrationAfter filtration
10. concentrationthe filtrate was concentrated
11. concentrationThe resulting concentrate
12. additionwas dispersed
13. washwashed by addition of n-hexane (500 ml)
14. customdried overnight under reduced pressure