HRID1492365

反应详情

EQUATION

反应方程式

HRID 1492365 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 2,6-dichloro-4-nitropyridine (3.8 g; 0.02 mol) in dimethylformamide (50 ml) cooled with an ice-bath was sodium thiomethoxide (1.4 g; 0.02 mol) slowly added. After stirring for 3 hours, the reaction mixture was quenched with water (300 ml) and extracted 3 times each with a hexane/ethyl acetate mixture (100 ml; 1/1). The combined extracts were dried with anhydrous magnesium sulphate and the solvent was removed in vacuo. Purification by silica gel flash column chromatography afforded 2,6-dichloro-4-methylthiopyridine (2.9 g; 74%) as a colorless oil.

WORKUP

后处理

  1. additionslowly added
  2. customthe reaction mixture was quenched with water (300 ml)
  3. extractionextracted 3 times each with a hexane/ethyl acetate mixture (100 ml; 1/1)
  4. dry with materialThe combined extracts were dried with anhydrous magnesium sulphate
  5. customthe solvent was removed in vacuo
  6. customPurification by silica gel flash column chromatography