HRID1675128

反应详情

EQUATION

反应方程式

HRID 1675128 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

Ethyl 3-(pyridin-4-yl)benzoate (1.46 g, 6.42 mmol), 5% palladium on carbon (50% wet) (0.301 g, 0.07 mmol) and citric acid monohydrate (0.601 g, 2.86 mmol) in a mixture of isopropanol (50 mL) and water (5 mL) were stirred under an atmosphere of hydrogen at 20 atmosphere and 70° C. for 15 hours. The reaction was cooled to room temperature, the catalyst removed by filtration and the solvent evaporated to give the crude product, which was purified by ion exchange chromatography, using an SCX column. The desired product was eluted from the column using 2M ammonia in methanol to give ethyl 3-(piperidin-4-yl)benzoate (1.190 g, 79%) as a liquid.

WORKUP

后处理

  1. temperatureThe reaction was cooled to room temperature
  2. customthe catalyst removed by filtration
  3. customthe solvent evaporated
  4. customto give the crude product, which
  5. customwas purified by ion exchange chromatography
  6. washThe desired product was eluted from the column