反应详情

温度

90 °C

A mixture of 2-bromo-4-fluoro-benzoic acid methyl ester (2.06 g, 8.84 mmol), 4-hydroxy piperidine (1.86 g, 18.4 mmol), and potassium carbonate (1.33 g, 9.62 mmol) in acetonitrile (25 mL) is heated to 90° C. for 17 h. The mixture is concentrated and partitioned between ethyl acetate and water. The solvent layers are separated and the aqueous layer is extracted with ethyl acetate (3×). The combined ethyl acetate layers are dried (MgSO4), filtered, and concentrated under reduced pressure. The residue is purified on silica (120 g) using a gradient of 0% to 90% ethyl acetate in heptane to provide the title compound (2.10 g, 76%) LC-ES/MS m/z 314.0 (M+1)

1. concentrationThe mixture is concentrated
2. custompartitioned between ethyl acetate and water
3. customThe solvent layers are separated
4. extractionthe aqueous layer is extracted with ethyl acetate (3×)
5. dry with materialThe combined ethyl acetate layers are dried (MgSO4)
6. filtrationfiltered
7. concentrationconcentrated under reduced pressure
8. customThe residue is purified on silica (120 g)