反应详情

A mixture of ethyl 1-(4-methoxybenzyl)-2-oxo-3-(3,4,5-trifluorophenoxy)piperidine-3-carboxylate (352 mg) and 1N aqueous sodium hydroxide solution (1.6 mL) in THF (3 mL) was stirred at room temperature for 2 days, and acidified with 1N hydrochloric acid, and extracted with ethyl acetate. The organic layer was separated, washed with saturated brine, and dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. The residue was recrystallized from ethyl acetate/hexane, the white crystals were separated by filtration, and the filtrate was concentrated. A mixture of the residue and the white crystals in toluene (3 mL) was stirred at 100° C. for 1 hr, and the solvent was evaporated under reduced pressure to give the title compound (252 mg).

1. extractionextracted with ethyl acetate
2. customThe organic layer was separated
3. washwashed with saturated brine
4. dry with materialdried over anhydrous magnesium sulfate
5. customthe solvent was evaporated under reduced pressure
6. customThe residue was recrystallized from ethyl acetate/hexane
7. customthe white crystals were separated by filtration
8. concentrationthe filtrate was concentrated
9. additionA mixture of the residue
10. stirringthe white crystals in toluene (3 mL) was stirred at 100° C. for 1 hr
11. customthe solvent was evaporated under reduced pressure