Reaktion #568937

Reaktionsgleichung

triethylamine

4,4'-dibromo-2,2-bipyridine

DCM MeOH

diethylphosphite

→

diethyl-4-bromo-2,2'-bipyridine-4'-phosphonate

Lösungsmittel

methanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONfilled 50 ml round bottom
2. 2
   Sonstigeflask, equipped with a cold finger (10 cm) and magnetic stirrer
3. 3
   TemperaturThis is then cooled back to room temperature
4. 4
   Sonstigeevaporated to dryness under reduced pressure

Vorschrift

2.0 g of 4,4'-dibromo-2,2-bipyridine (6.4 mmol), 0.9g of palladium tetrakistriphenylphosphine (0.8 mmol), 3.14 g of diethylphosphite (23 mmol) and 2.34 g of triethylamine (23 mmol) are measured into an argon filled 50 ml round bottom. flask, equipped with a cold finger (10 cm) and magnetic stirrer. This is heated on a 98° C. oil bath for 3 hours. The reaction is monitored with TLC on silica gel plates, DCM: MeOH (10:1), Rf-Lb=0.73. This is then cooled back to room temperature, and then the solidified mixture is added to 25 mls of methanol, stirred for 10 min. and evaporated to dryness under reduced pressure.

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