반응 #1584541

반응 방정식

5-bromo-2-ethyl-3-methyl-2H-indazole

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

potassium carbonate

trans-N,N′-dimethylcyclohexane-1,2-diamine

→

title compound

수율 13.6%

4-[(4-chlorobenzyl)oxy]-1-(2-ethyl-3-methyl-2H-indazol-5-yl)pyridin-2(1H)-one

수율 13.6%

용매

1,4-dioxane

반응 조건

후처리

1. 1
   온도The reaction mixture was cooled to room temperature
2. 2
   농축concentrated under reduced pressure
3. 3
   workup.ADDITIONTo the residue were added dichloromethane and water
4. 4
   세척the organic layer was washed with saturated brine
5. 5
   건조dried over anhydrous sodium sulfate
6. 6
   농축concentrated under reduced pressure
7. 7
   기타The obtained residue was purified by silica gel column chromatography (dichloromethane/methanol)

실험 절차

To a solution of 5-bromo-2-ethyl-3-methyl-2H-indazole (200 mg), 4-[(4-chlorobenzyl)oxy]pyridin-2(1H)-one (158 mg) and potassium carbonate (347 mg) in 1,4-dioxane (10 ml) were added copper(I) iodide (64 mg) and trans-N,N′-dimethylcyclohexane-1,2-diamine (47 mg), and the mixture was stirred at 110° C. for 16 hr. The reaction mixture was cooled to room temperature, and concentrated under reduced pressure. To the residue were added dichloromethane and water, and the organic layer was washed with saturated brine, dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The obtained residue was purified by silica gel column chromatography (dichloromethane/methanol) to give the title compound (36 mg).

출처