反应详情

温度

50 °C

Ethyl 7-(2-{[di-tert-butyl(phenyl)silyl]oxy}-1-methylethoxy)-5-[4-(methylsulfonyl)phenoxy]-1H-indole-2-carboxylate (2.4 g) was dissolved in a mixed solvent of tetrahydrofuran (10 mL)-ethanol (10 mL), 1M aqueous sodium hydroxide solution (5 mL) was added, and the mixture was stirred at 50° C. for 1 hr. 1M Aqueous sodium hydroxide solution (1 mL) was added to the reaction solution, and the mixture was stirred at 50° C. for 40 min. 1M Aqueous sodium hydroxide solution (1 mL) was added again, and the mixture was further stirred at 50° C. for 30 min. The reaction solution was allowed to cool to room temperature, and concentrated under reduced pressure. Water was added to the residue, and the mixture was neutralized with 1M hydrochloric acid, and subjected to extraction with ethyl acetate. The organic layer was washed with saturated brine, dried over magnesium sulfate, filtrated, and concentrated under reduced pressure to give the title compound (1.9 g, yield 83%) as a pale-red amorphous solid. MS 644 (MH+).

1. additionwas added
2. stirringthe mixture was stirred at 50° C. for 40 min
3. stirringthe mixture was further stirred at 50° C. for 30 min
4. temperatureto cool to room temperature
5. concentrationconcentrated under reduced pressure
6. additionWater was added to the residue
7. extractionsubjected to extraction with ethyl acetate
8. washThe organic layer was washed with saturated brine
9. dry with materialdried over magnesium sulfate
10. filtrationfiltrated
11. concentrationconcentrated under reduced pressure