HRID273326

反应详情

EQUATION

反应方程式

HRID 273326 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Methylzinc chloride in THF (2 M, 10.489 mL, 21 mmol) was added to a solution of 2-chloro-4-methoxypyridine (0.500 g, 3.48 mmol) and Pd(PPh3)4 (0.161 g, 0.14 mmol) in THF (10 mL). The mixture was refluxed for 40 h and then poured into an aqueous solution (10 mL) containing ethylenediaminetetraacetic acid (1.5 g). The resulting mixture was neutralized with K2CO3 and extracted with Et2O. The organic layer was concentrated to give a residue, which was purified on a silica gel column eluting with MeOH:EtOAc (1:10) to give 4-methoxy-2-methylpyridine (0.213 g, 50.0%).

WORKUP

后处理

  1. temperatureThe mixture was refluxed for 40 h
  2. extractionextracted with Et2O
  3. concentrationThe organic layer was concentrated
  4. customto give a residue, which
  5. customwas purified on a silica gel column
  6. washeluting with MeOH:EtOAc (1:10)