반응 #1136607

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sodium hydrogen carbonate

ethyl 3-cyclopropyl-3-(3-((N-(2′-fluoro-5′-methoxy-2-neopentyl-[1,1′-biphenyl]-4-yl)-2-nitrophenylsulfonamido)methyl)phenyl)propanoate

mercaptoacetic acid

lithium hydroxide monohydrate

→

title compound

수율 89.1%

ethyl 3-cyclopropyl-3-(3-(((2′-fluoro-5′-methoxy-2-neopentyl-[1,1′-biphenyl]-4-yl)amino)methyl)phenyl)propanoate

수율 89.1%

용매

DMF

반응 조건

후처리

1. 1
   추출the mixture was extracted with ethyl acetate
2. 2
   세척The extract was washed with saturated brine
3. 3
   건조dried over anhydrous sodium sulfate
4. 4
   기타The solvent was evaporated under reduced pressure
5. 5
   기타the residue was purified by silica gel column chromatography (NH, ethyl acetate/hexane)

실험 절차

To a solution of ethyl 3-cyclopropyl-3-(3-((N-(2′-fluoro-5′-methoxy-2-neopentyl-[1,1′-biphenyl]-4-yl)-2-nitrophenylsulfonamido)methyl)phenyl)propanoate (1.22 g) in DMF (35 mL) were added mercaptoacetic acid (617 μL) and lithium hydroxide monohydrate (728 mg) at room temperature, and the mixture was stirred at 60° C. for 1 hr. To the reaction mixture was added saturated aqueous sodium hydrogen carbonate solution at 0° C., and the mixture was extracted with ethyl acetate. The extract was washed with saturated brine and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure and the residue was purified by silica gel column chromatography (NH, ethyl acetate/hexane) to give the title compound (801 mg) as a colorless oil.

출처