反应详情

温度

100 °C

4-(4-Benzylpiperazin-1-yl)benzonitrile (4.0 g, 15 mmol) was dissolved in glacial acetic acid (40 mL), 6 M hydrochloric acid (50 mL) was added and the reaction mixture was stirred at 100° C. for 17 h. The solvent was evaporated, the residue was suspended in water (10 mL) and the pH was adjusted to 3 by addition of 2 M sodium hydroxide (35 ml). The slurry was stirred at 50° C. for 2 h, cooled and the precipitate was filtered and dried in vacuo to give 4.1 g of a crude product. The solid was partitioned between methylene chloride (40 mL) and water (220 mL) with 2 M sodium hydroxide (8 mL). The aqueous phase wag washed with methylene chloride (40 mL) and the pH was adjusted to 5 with 2 M hydrochloric acid. The aqueous phase was cooled, the precipitate was filtered and dried in vacuo to give 1.6 g (38% yield) of the title compound: mp 226° C. (dec); EIMS (70 eV) m/z (relative intensity) 296 (44, M30 ).

1. customThe solvent was evaporated
2. additionthe pH was adjusted to 3 by addition of 2 M sodium hydroxide (35 ml)
3. stirringThe slurry was stirred at 50° C. for 2 h
4. temperaturecooled
5. filtrationthe precipitate was filtered
6. customdried in vacuo
7. customto give 4.1 g of a crude product
8. customThe solid was partitioned between methylene chloride (40 mL) and water (220 mL) with 2 M sodium hydroxide (8 mL)
9. washThe aqueous phase wag washed with methylene chloride (40 mL)
10. temperatureThe aqueous phase was cooled
11. filtrationthe precipitate was filtered
12. customdried in vacuo