반응 #1584577

반응 방정식

N,N′-dimethylethylenediamine

5-bromo-4-fluoro-2,3-dimethyl-2H-indazole

4-[(4-chlorobenzyl)oxy]pyridin-2(1H)-one

potassium carbonate

ammonia

→

title compound

수율 2.9%

4-[(4-chlorobenzyl)oxy]-1-(4-fluoro-2,3-dimethyl-2H-indazol-5-yl)pyridin-2(1H)-one

수율 2.9%

용매

DMSO

반응 조건

후처리

1. 1
   기타the mixture was reacted at 150° C. for 1 hr under microwave irradiation
2. 2
   추출the mixture was extracted with ethyl acetate
3. 3
   세척The organic layer was washed with saturated brine
4. 4
   건조dried over anhydrous magnesium sulfate
5. 5
   농축concentrated under reduced pressure
6. 6
   기타The obtained residue was purified by silica gel column chromatography (ethyl acetate/methanol)
7. 7
   기타recrystallized from ethyl acetate

실험 절차

To a suspension of 5-bromo-4-fluoro-2,3-dimethyl-2H-indazole (142 mg), 4-[(4-chlorobenzyl)oxy]pyridin-2(1H)-one (138 mg) and potassium carbonate (242 mg) in DMSO (3 ml) were added copper(I) iodide (111 mg) and N,N′-dimethylethylenediamine (103 mg) at room temperature, and the mixture was reacted at 150° C. for 1 hr under microwave irradiation. The reaction mixture was added to 28% aqueous ammonia, and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated brine, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The obtained residue was purified by silica gel column chromatography (ethyl acetate/methanol) and recrystallized from ethyl acetate to give the title compound (6.8 mg).

출처