反应详情

To a round-bottomed flask equipped with stirring was added (methylsulfonyl){2-[4-benzylpiperazinyl]phenyl}amine (42 g, 120 mmol), MeOH, 10% Pd/C (Aldrich) (25 g), and HCO2NH4 (38 g, 610 mmol) After heating at reflux for 2 h, the mixture was filtered through Celite® and washed with CH2Cl2. The combined organic layers were washed with NaHCO3 and concentrated in vacuo to afford a light yellow solid. This was treated with a soln of EtOAc and HCl to afford the salt of the desired compound as the hydrochloride salt (20 g). MS (ESI, pos. Ion) m/z: 256 (M+H); MS (ESI, neg. Ion) m/z: 254 (M−H). Calc'd for C11H17N3O2S: 255.10.

1. customTo a round-bottomed flask equipped
2. temperatureAfter heating
3. temperatureat reflux for 2 h
4. filtrationthe mixture was filtered through Celite®
5. washwashed with CH2Cl2
6. washThe combined organic layers were washed with NaHCO3
7. concentrationconcentrated in vacuo
8. customto afford a light yellow solid