HRID964006

反应详情

EQUATION

反应方程式

HRID 964006 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A suspension of 4-carbamoyl-1-(3-methoxyphenyl)-pyridinium chloride (26 g) in methanol (300 ml) was hydrogenated at ambient temperature and pressure in the presence of 10% palladium-on-carbon catalyst (2.0 g) until hydrogen uptake ceased (~2 days) The mixture was filtered, excess triethylamine added and the solvent removed in vacuo to give a pink solid. This was partitioned between water and chloroform. The organic phase was dried and the solvent removed in vacuo to give 1-(3-methoxyphenyl)piperidine-4-carboxamide as a pink solid (19 g), m.p. 153°-156° C.

WORKUP

后处理

  1. customwas hydrogenated at ambient temperature
  2. custom(~2 days)
  3. filtrationwas filtered
  4. additionexcess triethylamine added
  5. customthe solvent removed in vacuo
  6. customto give a pink solid
  7. customThis was partitioned between water and chloroform
  8. customThe organic phase was dried
  9. customthe solvent removed in vacuo