反应详情

温度

60 °C

To methyl 1-(biphenyl-4-ylmethyl)-1H-indole-7-carboxylate (2.5 g) were added methanol (20 mL), THF (20 mL), and a 1 M aqueous sodium hydroxide solution (10 mL), followed by stirring at 60° C. for 16 hours. To the reaction mixture was added a 10% aqueous citric acid solution (20 mL), followed by extraction with ethyl acetate, and the organic layer was washed with brine. After dehydration over anhydrous sodium sulfate, filtering and concentrating under reduced pressure, the obtained residue was added with diisopropylether, solidified, and collected by filtration. This solid was purified by silica gel column chromatography (chloroform/methanol=99/1-97/3) to obtain 1-(biphenyl-4-ylmethyl)-1H-indole-7-carboxylic acid (0.99 g).

1. extractionfollowed by extraction with ethyl acetate
2. washthe organic layer was washed with brine
3. filtrationAfter dehydration over anhydrous sodium sulfate, filtering
4. concentrationconcentrating under reduced pressure
5. additionthe obtained residue was added with diisopropylether
6. filtrationcollected by filtration
7. customThis solid was purified by silica gel column chromatography (chloroform/methanol=99/1-97/3)