반응 #59044

반응 방정식

benzyl 4′-{2-[(1S,2R)-2-hydroxy-2-(4-hydroxyphenyl)-1-methylethylamino]ethoxy}-3′,5′-dimethylbiphenyl-4-carboxylate

→

title compound

수율 27.9%

4′-{2-[(1S,2R)-2-Hydroxy-2-(4-hydroxyphenyl)-1-methylethylamino]ethoxy}-3′,5′-dimethylbiphenyl-4-carboxylic acid

수율 27.9%

용매

N,N-dimethylformamide

반응 조건

후처리

1. 1
   기타The catalyst was removed by filtration
2. 2
   농축the filtrate was concentrated in vacuo
3. 3
   workup.ADDITIONMethylene chloride was added to the residue
4. 4
   여과The resulting precipitate was collected by filtration
5. 5
   기타purified by octadecyl silica gel column chromatography (eluent:acetonitrile/water=1/1)

실험 절차

A mixture of benzyl 4′-{2-[(1S,2R)-2-hydroxy-2-(4-hydroxyphenyl)-1-methylethylamino]ethoxy}-3′,5′-dimethylbiphenyl-4-carboxylate (0.108 g) and 10% palladium-carbon (50% wet, 0.05 g) in N,N-dimethylformamide (4 mL) was stirred at room temperature for 1.5 hrs under an atmosphere of hydrogen. The catalyst was removed by filtration, and the filtrate was concentrated in vacuo. Methylene chloride was added to the residue. The resulting precipitate was collected by filtration, and purified by octadecyl silica gel column chromatography (eluent:acetonitrile/water=1/1) to afford the title compound (0.025 g) as a white amorphous. The structure and physical data were shown in table 1.

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