反应详情

温度

60 °C

Aq. 1M LiOH (15.0 mL, 15.0 mmol) was added to a sol. of compound C7 (2.04 g, 3.64 mmol) in THF (15 mL). The mixture was stirred at 60° C. for 3 days, and aq. 1M HCl was added. The mixture was extracted with EtOAc (2×). The combined org. extracts were washed with aq. 1M HCl and brine, dried over MgSO4, filtered, and the solvents were removed under reduced pressure. Purification of the crude by FC (EtOAc) yielded the crude title compound mixed with 4-{4-[3-(2-chloro-3,6-difluoro-phenyl)-isoxazol-5-ylmethoxy]-phenyl}-3,6-dihydro-2H-pyridine-1,3-dicarboxylic acid 1-tert-butyl ester (600 mg, 30%). LC-MS: tR=1.08 min; ES+: 547.20.

1. extractionThe mixture was extracted with EtOAc (2×)
2. washextracts were washed with aq. 1M HCl and brine
3. dry with materialdried over MgSO4
4. filtrationfiltered
5. customthe solvents were removed under reduced pressure
6. customPurification of the crude by FC (EtOAc)