反应详情

To a stirred solution of 3-chloro-2-[(2R,6S)-2,6-dimethylmorpholin-4-yl]-4-fluorobenzoic acid (Intermediate 35, 10.0 g, 34.8 mmol) in methanol (50 mL) was added concentrated H2SO4 (1 mL) and the solution was refluxed for 12 hours. The reaction mixture was concentrated and diluted with EtOAc (100 mL). The organic layer washed with H2O (2×20 mL), dried over anhydrous sodium sulfate and concentrated. The residue was purified by column chromatography with ethyl acetate-pet. ether to give product as a solid. Yield: 9.0 g (86%)

1. temperaturethe solution was refluxed for 12 hours
2. concentrationThe reaction mixture was concentrated
3. additiondiluted with EtOAc (100 mL)
4. washThe organic layer washed with H2O (2×20 mL)
5. dry with materialdried over anhydrous sodium sulfate
6. concentrationconcentrated
7. customThe residue was purified by column chromatography with ethyl acetate-pet. ether
8. customto give product as a solid