HRID1368237

反应详情

EQUATION

反应方程式

HRID 1368237 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

PROCEDURE

实验过程

2,3-Diamino-6-bromopyridine (8.16 g) and triethyl orthoacetate (12.0 ml) were mixed in acetic acid (41 ml), and the mixture was refluxed under heating for 29 hr. After allowing to cool, the solvent was evaporated under reduced pressure to give a crude product (10 g). This was dissolved in a sufficient amount of dichloromethane and anhydrous potassium carbonate and active charcoal were added. The mixture was stirred at room temperature. The insoluble matter was removed by filtration and the solvent was evaporated to give 5-bromo-2-methyl-1H-imidazo[4,5-b]pyridine (7.59 g) as a pale-yellow powder.

WORKUP

后处理

  1. temperaturethe mixture was refluxed
  2. temperatureunder heating for 29 hr
  3. temperatureto cool
  4. customthe solvent was evaporated under reduced pressure
  5. customto give a crude product (10 g)
  6. additionwere added
  7. customThe insoluble matter was removed by filtration
  8. customthe solvent was evaporated