HRID578591

反应详情

EQUATION

反应方程式

HRID 578591 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

{circle around (1)} 100 g (0.676 mol) of 2,3-dichloropyridine, 91.87 g (0.676 mol) of p-tolylboronic acid, and 86 g (0.811 mol) of sodium carbonate were dissolved in 500 mL of 1,2-dimethoxyethane and 500 mL of distilled water, after which 78 g (0.0676 mol) of Pd(PPh3)4 was added. The mixture was heated to reflux for 18 hours so that it was allowed to react. After completion of the reaction, the reaction solution was concentrated under reduced pressure to remove 1,2-dimethoxyethane, and then extracted with ethyl acetate. The extract was treated with magnesium sulfate, filtered, and concentrated under reduced pressure, yielding 3-chloro-2-para-tolylpyridine as represented below in a 84% yield.

WORKUP

后处理

  1. temperatureThe mixture was heated
  2. temperatureto reflux for 18 hours so that it
  3. customto react
  4. customAfter completion of the reaction
  5. concentrationthe reaction solution was concentrated under reduced pressure
  6. customto remove 1,2-dimethoxyethane
  7. extractionextracted with ethyl acetate
  8. additionThe extract was treated with magnesium sulfate
  9. filtrationfiltered
  10. concentrationconcentrated under reduced pressure