HRID1389151

反应详情

EQUATION

反应方程式

HRID 1389151 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

4-(N-phenylcarbamoyl)pyridine [75.0 g, prepared as in Chem. Abs., 2013h (1958)] was hydrogenated in acetic acid (800 ml) using a platinum oxide catalyst at 50 p.s.i./30°. The catalyst was then removed by filtration, the solution evaporated, the residue basified to about pH 12 with sodium hydroxide, extracted with chloroform, and the organic extract discarded. The aqueous phase was evaporated to dryness, the residue boiled with chloroform, filtered and evaporated to leave 4-(N-phenylcarbamoyl)piperidine (17.0 g), m.p. 121°-127°. The hydrochloride salt, m.p. 231°-233°, was prepared in isopropanol from the free base and hydrogen chloride, and was recrystallised from isopropanol/ethyl acetate.

WORKUP

后处理

  1. custom30°
  2. customThe catalyst was then removed by filtration
  3. customthe solution evaporated
  4. extractionextracted with chloroform
  5. extractionthe organic extract
  6. customThe aqueous phase was evaporated to dryness
  7. filtrationfiltered
  8. customevaporated