反应详情

温度

150 °C

To a 250 mL pressure bottle equipped with magnetic stirring was added methyl 2-fluorobenzoate (Lancaster Synthesis Inc.) (3.0 g, 20 mmol), 1-benzylpiperazine (Aldrich) (3.8 g, 22 mmol) and K2CO3 (3.0 g, 22 mmol) in DMF (100 mL). The mixture was heated at 150° C. for 12 h. After cooling to RT the reaction was diluted with EtOAc (100 mL) and H2O was added. The organic layer was separated and washed with H2O, brine, dried over Na2SO4, filtered and concentrated in vacuo to afford a brown oil. The crude material was purified by column chromatography (4:1 hexanes-EtOAc) to give the title compound as a white foam (3.6 g). MS (ESI, pos. ion) m/z: 311 (M+H). Calc'd for C19H22N2O2: 310.17.

1. customTo a 250 mL pressure bottle equipped
2. temperatureAfter cooling to RT the reaction
3. additionwas added
4. customThe organic layer was separated
5. washwashed with H2O, brine
6. dry with materialdried over Na2SO4
7. filtrationfiltered
8. concentrationconcentrated in vacuo
9. customto afford a brown oil
10. customThe crude material was purified by column chromatography (4:1 hexanes-EtOAc)