HRID437241

反应详情

EQUATION

反应方程式

HRID 437241 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. temperatureheated
  2. temperatureunder reflux for 4 hours
  3. filtrationThe resulting mixture was filtered
  4. customthe filtrate evaporated almost to dryness
  5. additiontreated with water (100 ml.)
  6. filtrationThe colourless solid was filtered off
  7. washwashed with water
  8. customdried
  9. dissolutiondissolved in a small amount of ethanolic hydrogen chloride
  10. additiontreated with ether until crystallisation
  11. filtrationFiltration
  12. customdrying
  13. customgave 1.875 g