反应详情

To a round-bottomed flask equipped with stirring was added N,N-dimethyl{2-[4-benzylpiperazinyl]phenyl} carboxamide (Step 2) (420 mg, 1.3 mmol), MeOH (10 mL), 10% Pd/C (Aldrich) (138 mg), and HCO2NH4 (409 mg, 6.5 mmol), and the reaction mixture was heated at reflux for 2 h. The reaction mixture was filtered through Celite®, concentrated in vacuo, and redissolved in CH2Cl2 (20 mL). The reaction mixture was washed with a Na2CO3 (10%, 2×), H2O, brine, dried over Na2SO4, filtered and concentrated in vacuo yielding N,N-dimethyl(2-piperazinylphenyl)carboxamide (255 mg). MS (ESI, pos.ion) m/z: 234 (M+H). Calc'd for C13H19N3O: 233.31.

1. customTo a round-bottomed flask equipped
2. temperaturethe reaction mixture was heated
3. temperatureat reflux for 2 h
4. filtrationThe reaction mixture was filtered through Celite®
5. concentrationconcentrated in vacuo
6. dissolutionredissolved in CH2Cl2 (20 mL)
7. washThe reaction mixture was washed with a Na2CO3 (10%, 2×), H2O, brine
8. dry with materialdried over Na2SO4
9. filtrationfiltered
10. concentrationconcentrated in vacuo