反应详情

A mixture of N-[3-[4-(6-fluoro-1,2-benzisoxazol-3yl)-1-piperidinyl]-propyl]phthalimide (8.5 g, 21 mmol), hydrazine monohydrate (1.5 g, 30 mmol) in methanol (60 ml) was heated at reflux for 2 hours. At the end of the reaction, methanol was removed to leave a crude solid. To this was added water (60 ml), then the mixture was acidified with HCl to pH 1. The insolubles were filtered with the aid of a pad of Celite. The aqueous solution was basified with 50% NaOH, (pH 13), then extracted with dichloromethane. The combined dichloromethane solution was washed with brine, then dried to a colorless oil (4.5 g). The analytical sample (1.5 g) was prepared by treating the oil with HCl in ethanol at 0° C. The 1-(3-aminopropyl)-4-(6-fluoro-1,2-benzisoxazol-3-yl)piperidine dihydrochloride was obtained as white crystals, 2.03 g, m.p.=231°-234° C.

1. temperaturewas heated
2. temperatureat reflux for 2 hours
3. customwas removed
4. customto leave a crude solid
5. filtrationThe insolubles were filtered with the aid of a pad of Celite
6. extractionextracted with dichloromethane
7. washThe combined dichloromethane solution was washed with brine
8. dry with materialdried to a colorless oil (4.5 g)
9. customThe analytical sample (1.5 g) was prepared