HRID230774

反应详情

EQUATION

反应方程式

HRID 230774 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Palladium acetate (267 mg), 1,1′-bis(diphenylphosphino)ferrocene (1.3 g) and triethylamine (3.2 mL) were added to an ethanol-DMF mixed solvent (1/1, 20 mL) of 6-chloropyridin-3-ol (1.5 g), and stirred overnight in a carbon monoxide atmosphere (1 atmospheric pressure) at 50° C. Ethanol was evaporated off under reduced pressure from the reaction solution, water was added to the resulting residue, and extracted with chloroform/methanol (10/1). The organic layer was dried with anhydrous magnesium sulfate, and the solvent was evaporated off under reduced pressure. The resulting residue was purified through silica gel column chromatography (hexane/ethyl acetate=2/3) to obtain the entitled compound (500 mg).

WORKUP

后处理

  1. customEthanol was evaporated off under reduced pressure from the reaction solution, water
  2. additionwas added to the resulting residue
  3. extractionextracted with chloroform/methanol (10/1)
  4. dry with materialThe organic layer was dried with anhydrous magnesium sulfate
  5. customthe solvent was evaporated off under reduced pressure
  6. customThe resulting residue was purified through silica gel column chromatography (hexane/ethyl acetate=2/3)