HRID1815106

反应详情

EQUATION

反应方程式

HRID 1815106 的结构方程式

PROCEDURE

实验过程

3-Nitro-6-(methylthio)pyridine (22.0 g, 129.3 mmol) was dissolved in acetone (140 mL). Sulfuric acid (2N, 230 mL) was then added dropwise to above solution to form a slurry. Potassium permanganate (KMnO4) (26.5 g, 168.1 mmol, dissolved in 500 mL of H2O) was added to the above mixture dropwise. The mixture that resulted was stirred at room temperature overnight. The solid was filtered and stirred with a warm mixture of ethanol/methanol (10/1). The insoluble salt was filtered, the filtrate was concentrated to provide a pale yellow solid. The crude product was recrystallized from ethanol to furnish the title compound (17.8 g, 70%).

WORKUP

后处理

  1. customto form a slurry
  2. customThe mixture that resulted
  3. filtrationThe solid was filtered
  4. stirringstirred with a warm mixture of ethanol/methanol (10/1)
  5. filtrationThe insoluble salt was filtered
  6. concentrationthe filtrate was concentrated
  7. customto provide a pale yellow solid
  8. customThe crude product was recrystallized from ethanol