Reaktion #610281

Reaktionsgleichung

5-bromo-3-methoxypyridin-2-amine

1,2-dimethyl-1H-imidazole

KOAc

→

title compound

5-(1,2-Dimethyl-1H-imidazol-5-yl)-3-methoxypyridin-2-amine

Lösungsmittel

DMA

Reaktionsbedingungen

Aufarbeitung

1. 1
   FiltrationThe reaction mixture was filtered
2. 2
   workup.ADDITIONdiluted with NaCl solution
3. 3
   Extraktionextracted with EtOAc
4. 4
   SonstigeThe organic layer was purified
5. 5
   Waschenby eluting through an SCX-2 column
6. 6
   Wascheneluting with 0-12% MeOH/EtOAc

Vorschrift

A suspension of 5-bromo-3-methoxypyridin-2-amine (55.5 mg, 0.273 mmol), 1,2-dimethyl-1H-imidazole (52.6 mg, 0.547 mmol), Pd(OAc)2 (2.5 mg, 0.011 mmol), KOAc (53.7 mg, 0.55 mmol) in DMA (3 mL) was stirred at 150° C. under microwave irradiation for 8 hours. The reaction mixture was filtered, diluted with NaCl solution and extracted with EtOAc. The organic layer was purified by eluting through an SCX-2 column using 2M NH3/MeOH followed by Biotage silica gel column chromatography eluting with 0-12% MeOH/EtOAc to give the title compound as yellow waxy solid (9 mg, 15%).

Quelle