HRID228802

反应详情

EQUATION

反应方程式

HRID 228802 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

6-Fluoro-2-iodo-3-methoxypyridine (84 mg), tetrakistriphenylphosphine palladium (0) (38 mg), and copper(II) oxide (53 mg) were suspended in N,N-dimethylformamide (2 ml). 2-Tributylstannylpyridine (244 mg) was added to the suspension, and the mixture was stirred at 100° C. overnight. The reaction solution was cooled to room temperature. The reaction solution was then filtered, the solvent was removed from the filtrate by distillation under the reduced pressure. Water was then added to the residue, and the mixture was extracted with dichloromethane. The dichloromethane layer was washed with water and saturated brine and was dried over anhydrous magnesium sulfate. The solvent was removed by distillation under the reduced pressure, and the residue was purified by thin layer chromatography using chloroform-methanol to give 6-fluoro-3-methoxy-[2,2′]bipyridine (12 mg, yield 18%).

WORKUP

后处理

  1. temperatureThe reaction solution was cooled to room temperature
  2. filtrationThe reaction solution was then filtered
  3. customthe solvent was removed from the filtrate by distillation under the reduced pressure
  4. additionWater was then added to the residue
  5. extractionthe mixture was extracted with dichloromethane
  6. washThe dichloromethane layer was washed with water and saturated brine
  7. dry with materialwas dried over anhydrous magnesium sulfate
  8. customThe solvent was removed by distillation under the reduced pressure
  9. customthe residue was purified by thin layer chromatography