Reaktion #489388

Reaktionsgleichung

2-biphenylamine

2-bromobiphenyl

tert-butoxy sodium

→

dibiphenyl-2-yl amine

Ausbeute 71.0%

Lösungsmittel

toluene

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturwas cooled to room temperature
2. 2
   Waschenthe reactant mixture was washed
3. 3
   Sonstigeto separate an organic layer
4. 4
   WaschenThe separated organic layer was washed with distilled water three times
5. 5
   Trocknenwas then dried with magnesium sulfate
6. 6
   SonstigeThereafter, residues from which volatile components were removed at reduced pressure
7. 7
   Sonstigewere purified
8. 8
   Sonstigewere then recrystallized in normal hexane

Vorschrift

Trisdibenzylideneacetonedipalladium (0.276 g, 0.3 mmol) and tri-tert-butylphosphine (0.121 g, 0.6 mmol) were put into a flask, and then dissolved in 40 mL of toluene. Subsequently, 2-biphenylamine (2.53 g, 15 mmol), 2-bromobiphenyl (3.50 g, 15 mmol) and tert-butoxy sodium (2.16 g, 22.5 mmol) were added into the flask, and then refluxed at a temperature of 110° C. for 12 hours. After the flask including the reactant mixture was cooled to room temperature, the reactant mixture was washed using an ammonium chloride aqueous solution (150 mL) to separate an organic layer. The separated organic layer was washed with distilled water three times, and was then dried with magnesium sulfate. Thereafter, residues from which volatile components were removed at reduced pressure were purified using a silica gel chromatography tube in a mixed solvent of hexane and ethylacetate (1:10), and were then recrystallized in normal hexane to produce 3.42 g of dibiphenyl-2-yl amine.

Quelle