反应详情

To the obtained tert-butyl 2-(4-fluoroanilino)-4-((E)-2-(2-methoxyphenyl)vinyl)benzoate were added acetic acid 4.0 mL and 10% palladium-carbon 26 mg sequentially, and it was stirred under hydrogen atmosphere at room temperature for 7 hours. Subsequently, 10% palladium-carbon 39 mg was added to it, it was stirred under hydrogen atmosphere at the same temperature for 3 hours, subsequently it was stirred at 40° C. for 2 hours. After the reaction mixture was cooled to room temperature, insoluble matter was filtrated, 10% palladium-carbon 64 mg was added to it, and it was stirred under hydrogen atmosphere at 40° C. for 3 hours and 30 minutes. After the reaction mixture was cooled to room temperature, insoluble matter was filtrated, and the solvent was removed under reduced pressure. To the obtained residue were added water, ethyl acetate and saturated sodium hydrogen carbonate aqueous solution. The organic layer was separated and collected,dried over anhydrous magnesium sulfate after washing with saturated sodium chloride aqueous solution, and the solvent was removed under reduced pressure to give tert-butyl 2-(4-fluoroanilino)-4-(2-(2-methoxyphenyl)ethyl)benzoate 0.11 g of a pale red oil.

1. stirringwas stirred under hydrogen atmosphere at the same temperature for 3 hours
2. stirringsubsequently it was stirred at 40° C. for 2 hours
3. temperatureAfter the reaction mixture was cooled to room temperature
4. filtrationinsoluble matter was filtrated
5. addition10% palladium-carbon 64 mg was added to it, and it
6. stirringwas stirred under hydrogen atmosphere at 40° C. for 3 hours and 30 minutes
7. temperatureAfter the reaction mixture was cooled to room temperature
8. filtrationinsoluble matter was filtrated
9. customthe solvent was removed under reduced pressure
10. additionTo the obtained residue were added water, ethyl acetate and saturated sodium hydrogen carbonate aqueous solution
11. customThe organic layer was separated
12. washafter washing with saturated sodium chloride aqueous solution
13. customthe solvent was removed under reduced pressure