HRID1038578

反应详情

EQUATION

反应方程式

HRID 1038578 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

2-Methyl-5-[1-(phenylsulfonyl)cyclopropoxy]pyridine (540 mg, 1.87 mmol) was dissolved in methanol (5.5 mL), added sodium phosphite (671 mg, 5.598 mmol), and sodium amalgam (3.58 g, 7.47 mmol) under ice-cold conditions, stirred at the same temperature for 30 minutes, and then stirred at room temperature for 3 hours. The reaction solution was added a saturated aqueous solution of sodium hydrogen carbonate, and extracted with diethylether. The organic layer was washed with brine, dried over anhydrous sodium sulfate, and concentrated in vacuo. The obtained residue was purified by distillation, and the title compound (240 mg (yield 86%)) was obtained as a yellow oil.

WORKUP

后处理

  1. stirringstirred at room temperature for 3 hours
  2. extractionextracted with diethylether
  3. washThe organic layer was washed with brine
  4. dry with materialdried over anhydrous sodium sulfate
  5. concentrationconcentrated in vacuo
  6. distillationThe obtained residue was purified by distillation