HRID1963700

反应详情

EQUATION

反应方程式

HRID 1963700 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To ethylpiperidine-4-carboxylate (1 eq) in ethanol was added iodoethane (1.1 eq) and potassium carbonate (2 eq) and the resulting mixture was refluxed for 16 h. The mixture was then cooled to room temperature and filtered. Ethanol was concentrated and partitioned between methylene chloride and water. The organic layer was then washed with saturated sodium chloride solution, dried with sodium sulfate and concentrated. To it was then added concentrated hydrochloric acid and water (2:1) and the mixture was refluxed for 5 h. The resulting 1-(ethyl)piperidine-4-carboxylic acid was then azeotroped with toluene. MS: MH+=158.

WORKUP

后处理

  1. temperaturethe resulting mixture was refluxed for 16 h
  2. filtrationfiltered
  3. concentrationEthanol was concentrated
  4. custompartitioned between methylene chloride and water
  5. washThe organic layer was then washed with saturated sodium chloride solution
  6. dry with materialdried with sodium sulfate
  7. concentrationconcentrated
  8. additionTo it was then added concentrated hydrochloric acid and water (2:1)
  9. temperaturethe mixture was refluxed for 5 h
  10. customThe resulting 1-(ethyl)piperidine-4-carboxylic acid was then azeotroped with toluene