反应详情

温度

60 °C

Aq. 1M LiOH (11.1 mL, 11.1 mmol) was added to a sol. of compound C3 (1.50 g, 2.72 mmol) in THF (10 mL). The mixture was stirred at 60° C. for 3 days. The mixture was allowed to cool to rt, and aq. 1M HCl was added, until the mixture was acidic. The mixture was extracted with EtOAc. The 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 (heptane/EtOAc 1:2) yielded the title compound mixed with 4-{4-[2-(2,6-dichloro-4-methyl-phenoxy)-ethoxy]-phenyl}-3,6-dihydro-2H-pyridine-1,3-dicarboxylic acid 1-tert-butyl ester (1.41 g, 99%). LC-MS: tR=1.10 min; ES+: 522.30.

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