HRID49808

反应详情

EQUATION

反应方程式

HRID 49808 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
110 °C

PROCEDURE

实验过程

A mixture of 3-fluoronitrobenzene (10.0 g, 70.9 mmol) and piperidine (14 ml, 141 mmol) was stirred at 110° C. for 3 days. After cooling water (200 ml) was added and the mixture was extracted with dichloromethane (3×100 ml). The combined organic extracts were washed with saturated aqueous sodium carbonate, dried over sodium sulfate and evaporated to dryness to leave 1-(3-nitrophenyl)piperidine (13.7 g, 93%) as an oil. This oil was dissolved in ethanol (150 ml) and was hydrogenated at ambient pressure using palladium on activated carbon as the catalyst to yield 2a (11.7 g, 100%) as an oil.

WORKUP

后处理

  1. additionwas added
  2. extractionthe mixture was extracted with dichloromethane (3×100 ml)
  3. washThe combined organic extracts were washed with saturated aqueous sodium carbonate
  4. dry with materialdried over sodium sulfate
  5. customevaporated to dryness