反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
4-Benzamido-(4-phenyl-4-oxobutyl)piperidine (3.4 g.) was dissolved in methanol (125 ml.) and a solution of sodium borohydride (6.0 g.) in 0.2 N sodium hydroxide (30 ml.) was added at room temperature over a period of 0.5 hours. The resulting mixture was stirred for a further 2 hours and then heated under reflux for 4 hours. The resulting mixture was filtered, the filtrate evaporated almost to dryness and then treated with water (100 ml.). The colourless solid was filtered off, washed with water, dried, dissolved in a small amount of ethanolic hydrogen chloride and treated with ether until crystallisation commenced. Filtration and drying gave 1.875 g. of the hydrochloride of the title compound, m.p. 221° C. (Found: C, 68.1; H, 7.4; N, 7.3. C22H28N2O2.HCl requires C, 67.9; H, 7.5; N, 7.2%).
WORKUP
后处理
- temperatureheated
- temperatureunder reflux for 4 hours
- filtrationThe resulting mixture was filtered
- customthe filtrate evaporated almost to dryness
- additiontreated with water (100 ml.)
- filtrationThe colourless solid was filtered off
- washwashed with water
- customdried
- dissolutiondissolved in a small amount of ethanolic hydrogen chloride
- additiontreated with ether until crystallisation
- filtrationFiltration
- customdrying
- customgave 1.875 g