HRID484779

反应详情

EQUATION

反应方程式

HRID 484779 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A Paar shaker bottle was charged with 0.2 g (0.85 mmol) of 4-(4-chloro-3-nitrophenyl)pyridine, 0.07 g (0.85 mmol) of sodium acetate, 0.02 g of 5% palladium-on-carbon, and 3 ml of glacial acetic acid. It was then charged with hydrogen to 40 psi, and the shaker was turned on. The reaction mixture was heated to 60°-70° C. and maintained at that temperature for two hours, after which the reaction was stopped and the catalyst removed by filtration. To the filtrate was added water and then 50% aqueous caustic to a pH greater than 7. The reaction mixture was extracted with methylene chloride. The methylene chloride fraction was washed, dried, and evaporated. Analysis of the reaction mixture showed that the process resulted in an 83% yield of 4-(3-aminophenyl)pyridine.

WORKUP

后处理

  1. temperatureThe reaction mixture was heated to 60°-70° C.
  2. temperaturemaintained at that temperature for two hours
  3. customthe catalyst removed by filtration
  4. additionTo the filtrate was added water
  5. extractionThe reaction mixture was extracted with methylene chloride
  6. washThe methylene chloride fraction was washed
  7. customdried
  8. customevaporated