반응 #796964

반응 방정식

(6-(2-fluoro-5-methoxyphenyl)-5-neopentylpyridin-3-yl)methanol

methyl 3-cyclopropyl-3-(3-hydroxyphenyl)propanoate

1,1′-(azodicarbonyl)dipiperidine

tributylphosphine

→

title compound

수율 86.4%

methyl 3-cyclopropyl-3-(3-((6-(2-fluoro-5-methoxyphenyl)-5-neopentylpyridin-3-yl)methoxy)phenyl)propanoate

수율 86.4%

용매

toluene

Hexane ethyl acetate

반응 조건

후처리

1. 1
   여과the resulting precipitate was filtered off
2. 2
   기타The solvent in the filtrate was evaporated under reduced pressure
3. 3
   기타the residue was purified by silica gel column chromatography (ethyl acetate/hexane)

실험 절차

Under a nitrogen atmosphere, to a solution of (6-(2-fluoro-5-methoxyphenyl)-5-neopentylpyridin-3-yl)methanol (100 mg) and methyl 3-cyclopropyl-3-(3-hydroxyphenyl)propanoate (73 mg) in toluene (4.7 mL) were added 1,1′-(azodicarbonyl)dipiperidine (133 mg) and tributylphosphine (130 μL), and the mixture was stirred at room temperature for 60 hr. Hexane/ethyl acetate (1:1) was added to the reaction mixture, and the resulting precipitate was filtered off. The solvent in the filtrate was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography (ethyl acetate/hexane) to give the title compound (144 mg) as a colorless oil.

출처