HRID910613

反应详情

EQUATION

反应方程式

HRID 910613 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

Acetic acid (10 mL) and aqueous 30% hydrogen peroxide (452 μL) were added to methyl 4-pyridin-3-ylbenzoate (708 mg), followed by stirring at 70° C. for 18 hours. The reaction mixture was concentrated under reduced pressure, an aqueous saturated sodium hydrogencarbonate solution was added, followed by extraction with chloroform. The organic layer was dried over anhydrous sodium sulfate, the solvent was evaporated under reduced pressure, and the resulting residue was purified by silica gel column chromatography (methanol/chloroform=0% to 10%) to obtain methyl 4-(1-oxidopyridin-3-yl)benzoate (720 mg) as a white solid.

WORKUP

后处理

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. additionan aqueous saturated sodium hydrogencarbonate solution was added
  3. extractionfollowed by extraction with chloroform
  4. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  5. customthe solvent was evaporated under reduced pressure
  6. customthe resulting residue was purified by silica gel column chromatography (methanol/chloroform=0% to 10%)