反应详情

温度

110 °C

The 4-dimethylamino compound was obtained in the following preparation in which the dimethylamino group was derived from in situ decomposition of the solvent DMF: A mixture of methyl 2-(1-tert-butoxycarbonylpiperidin-4-yloxy)-4-fluorobenzoate (6.45 g, 18.25 mmol), morpholine (8 g, 91.26 mmol), Cs2CO3 (11.8 g, 36.5 mmol), and DMF (10 mL) was heated 3 days at 110° C. The reaction mixture was poured into brine (100 mL) and extracted with EtOAc (3×100 mL). The combined extracts were washed with brine (3×200 mL), dried over MgSO4, and concentrated to an oil which was purified by chromatography on silica using 25% EtOAc in hexanes to give 4.1 g (59%) of product as a white solid.

1. extractionextracted with EtOAc (3×100 mL)
2. washThe combined extracts were washed with brine (3×200 mL)
3. dry with materialdried over MgSO4
4. concentrationconcentrated to an oil which
5. customwas purified by chromatography on silica using 25% EtOAc in hexanes