反应详情

温度

130 °C

To a solution of 1-fluoro-4-nitro-benzene (314 mg, 2.23 mmol) and 4-tert-butyl-piperazine (1 g, 3.34 mmol) in dioxane (15 mL) is added K2CO3 (1.65 mg, 11.9 mmol) and the reaction is stirred at 130° C. overnight. The solvent is evaporated under vacuum and the residue is partitioned between ethyl acetate and water. The organic layer is washed with brine, dried over MgSO4, filtered and concentrated to give a crude compound. Purification by silica gel column chromatography eluting with DCM followed by 99:1 DCM:NH3 (7M in MeOH) affords the title compound (348 mg, 55.4%). LCMS: Rt 3.87 min (99%).

1. customThe solvent is evaporated under vacuum
2. customthe residue is partitioned between ethyl acetate and water
3. washThe organic layer is washed with brine
4. dry with materialdried over MgSO4
5. filtrationfiltered
6. concentrationconcentrated
7. customto give a crude compound
8. customPurification by silica gel column chromatography
9. washeluting with DCM