反应详情

A 150-mL round-bottomed flask was charged with N-(((2R)-1,4-dibenzyl-2-piperazinyl)methyl)-N-phenylmethanesulfonamide (0.527 g, 1.172 mmol, step 2), AcOH (0.10 mL, 1.7 mmol), Pd (10 wt. % (dry basis) on activated carbon, wet, Degussa type, 0.528 g), EtOH (10 mL) and EtOAc (2 mL). The reaction mixture was evacuated under vacuum and refilled with hydrogen. The mixture was stirred under an atmosphere of hydrogen at room temperature for 4.5 h then at 50° C. for 12 h. The reaction mixture was filtered and the filtrate was concentrated and re-subjected to the reaction condition (Pd/C 0.683 g and EtOH 10 mL). The reaction mixture was evacuated under vacuum and refilled with hydrogen. The mixture was stirred under an atmosphere of hydrogen at 50° C. for 12 h. The reaction mixture was filtered through a pad of filter agent. The filtrate was concentrated to give N-phenyl-N-((2R)-2-piperazinylmethyl)methanesulfonamide (0.378 g) as a clear oil.

1. customThe reaction mixture was evacuated under vacuum
2. additionrefilled with hydrogen
3. waitat 50° C. for 12 h
4. filtrationThe reaction mixture was filtered
5. concentrationthe filtrate was concentrated
6. customThe reaction mixture was evacuated under vacuum
7. additionrefilled with hydrogen
8. stirringThe mixture was stirred under an atmosphere of hydrogen at 50° C. for 12 h
9. filtrationThe reaction mixture was filtered through a pad of filter agent
10. concentrationThe filtrate was concentrated