反应详情

A solution of this benzoyl piperidine (2.3 9), the above 4-[(4-fluorophenyl)(4-methylthien-2-yl)methylene]piperidine (3 g) and triethylamine (3 ml) in toluene was boiled under reflux for 5 h. Water was added to the cooled mixture, the layers were separated and the toluene layer was separated, washed with brine, dried over sodium sulphate and evaporated. The resultant oil (5.6 g) was dissolved in dichloromethane and chromatographed on silica. Elution with dichloromethane/ammonium hydroxide (1%) containing increasing amounts of methanol gave fractions that on evaporation gave the title compound (4.36 g). A solution of this compound in ether was treated with with an ethereal solution of hydrogen chloride. The precipitate was collected and dried to give the hydrochloride salt (3.6 g) m.p. 118-142° C.

1. temperatureunder reflux for 5 h
2. customthe layers were separated
3. customthe toluene layer was separated
4. washwashed with brine
5. dry with materialdried over sodium sulphate
6. customevaporated
7. dissolutionThe resultant oil (5.6 g) was dissolved in dichloromethane
8. customchromatographed on silica
9. washElution with dichloromethane/ammonium hydroxide (1%)
10. additioncontaining
11. temperatureincreasing amounts of methanol
12. customgave fractions that
13. customon evaporation