HRID1164514

反应详情

EQUATION

反应方程式

HRID 1164514 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

1-Methyl-1-(4-pyridylmethyl)-3-phenylurea (7.0 g) in glacial acetic acid (50 ml) was hydrogenated over platinum oxide at 60°/60 p.s.i. until uptake of hydrogen ceased. The catalyst was removed by filtration and the filtrate evaporated in vacuo. The resultant oil was basified with 5 N NaOH (to pH 12) and extracted with chloroform (2×50 ml). The combined extracts were dried (MgSO4) and evaporated with chloroform (2×50 ml). The combined extracts were dried (MgSO4) and evaporated to give 1-methyl-1-(4-piperidylmethyl)-3-cyclohexylurea as an oil (4.0 g). The n.m.r. and mass spectra were compatible with the required structure.

WORKUP

后处理

  1. customThe catalyst was removed by filtration
  2. customthe filtrate evaporated in vacuo
  3. extractionextracted with chloroform (2×50 ml)
  4. dry with materialThe combined extracts were dried (MgSO4)
  5. customevaporated with chloroform (2×50 ml)
  6. dry with materialThe combined extracts were dried (MgSO4)
  7. customevaporated