反应详情

温度

50 °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 mL9 nd water (220 mL) with 2 M sodium hydroxide (8 mL). The aqueous phase was 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, M+).

1. customThe solvent was evaporated
2. additionthe pH was adjusted to 3 by addition of 2 M sodium hydroxide (35 ml)
3. temperaturecooled
4. filtrationthe precipitate was filtered
5. customdried in vacuo
6. customto give 4.1 g of a crude product
7. customThe solid was partitioned between methylene chloride (40 mL9 nd water (220 mL) with 2 M sodium hydroxide (8 mL)
8. washThe aqueous phase was washed with methylene chloride (40 mL)
9. temperatureThe aqueous phase was cooled
10. filtrationthe precipitate was filtered
11. customdried in vacuo