反应详情

温度

100 °C

A mixture of 1-(3-aminopropyl)-4-benzhydrylpiperazine (1.55 g) and acetic anhydride (16 ml) was stirred at 100° C. for 1.5 hours. The reaction mixture was concentrated and the residue was extracted with ethyl acetate. The extract was washed successively with aqueous sodium bicarbonate and water, dried and evaporated in vacuo. The residue was purified by column chromatography on silica gel eluting with ethyl acetate. The fractions containing the desired compound were combined and evaporated in vacuo to give a residue. According to a conventional manner, the residue was converted to hydrochloric acid salt, which was recrystallized from a mixture of methanol and diethyl ether to afford 1-(3-acetylaminopropyl)-4-benzhydrylpiperazine (0.8 g) as white crystals. mp: 240°-255° C. (dec.)

1. concentrationThe reaction mixture was concentrated
2. extractionthe residue was extracted with ethyl acetate
3. washThe extract was washed successively with aqueous sodium bicarbonate and water
4. customdried
5. customevaporated in vacuo
6. customThe residue was purified by column chromatography on silica gel eluting with ethyl acetate
7. additionThe fractions containing the desired compound
8. customevaporated in vacuo
9. customto give a residue
10. customwas recrystallized from a mixture of methanol and diethyl ether