Reaktion #41913

Reaktionsgleichung

tri-tert-butylphosphine

tris(2-bromo-6-pyridyl)phosphine oxide

2-methoxybenzeneboronic acid

potassium fluoride

→

Tris(6-(2-methoxyphenyl)-2-pyridyl)phosphine oxide

Lösungsmittel

water

ethyl acetate

THF

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturunder reflux for 16 h
2. 2
   TemperaturAfter cooling
3. 3
   SonstigeThe organic phase was removed
4. 4
   Waschenwashed twice with 500 ml of water and once with 500 ml of sat. sodium chloride solution
5. 5
   Trocknensubsequently dried over magnesium sulfate
6. 6
   EinengenAfter the organic phase had been concentrated under reduced pressure (end pressure 1 mbar, temperature 90° C.), 44.3 g (98.5%) of a pale yellow highly viscous oil
7. 7
   Sonstigewhich was reacted further without purification

Vorschrift

An efficiently stirred suspension of 38.8 g (75.0 mmol) of tris(2-bromo-6-pyridyl)phosphine oxide, 51.3 g (337.5 mmol) of 2-methoxybenzeneboronic acid and 43.1 g (742.5 mmol) of potassium fluoride in 750 ml of anhydrous THF was admixed with 593 mg (2.93 mmol) of tri-tert-butylphosphine and then with 505 mg (2.25 mmol) of palladium(II) acetate, and subsequently heated under reflux for 16 h. After cooling, the reaction mixture was admixed with 1500 ml of ethyl acetate and 1000 ml of water. The organic phase was removed, washed twice with 500 ml of water and once with 500 ml of sat. sodium chloride solution, and subsequently dried over magnesium sulfate. After the organic phase had been concentrated under reduced pressure (end pressure 1 mbar, temperature 90° C.), 44.3 g (98.5%) of a pale yellow highly viscous oil remained, which was reacted further without purification.

Quelle