HRID2373683

反应详情

EQUATION

反应方程式

HRID 2373683 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2-[(2-methoxyethyl)oxy]-6-methyl-4-methylthio-3-nitropyridine (2.00 g, 7.74 mmol) was dissolved in dichloromethane (25 mL). m-Chloroperbenzoic acid (60%, 5.0 g, 17.38 mmol) was added to the solution, followed by stirring at room temperature for 12 hours. Saturated aqueous sodium sulfite was added to the reaction mixture, followed by stirring for 1.5 hours so that excessive m-chloroperbenzoic acid was deactivated. The organic layer was washed with saturated brine, followed by drying over sodium sulfate anhydrate and concentration under reduced pressure. The obtained residue was recrystallized from ether, to thereby yield 2-[(2-methoxyethyl)oxy]-6-methyl-4-methylsulfinyl-3-nitropyridine as colorless crystals (1.93 g, 91%).

WORKUP

后处理

  1. washThe organic layer was washed with saturated brine
  2. dry with materialby drying over sodium sulfate anhydrate and concentration under reduced pressure
  3. customThe obtained residue was recrystallized from ether