HRID1471280

反应详情

EQUATION

反应方程式

HRID 1471280 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a flask were added 0.6 g pulverized potassium hydroxide and 15 ml dimethylsulfoxide. After adding 1.4 g of 2,2′-dipyridylamine, the mixture was stirred under nitrogen for 45 minutes, when 1.5 g 6-methyl-2-(bromomethyl)pyridine was added. After stirring for 1 hour, 35 ml of water was added and the product was extracted with 60 ml of 50% ethyl acetate, 50% hexane. The organic layer was washed with 30 ml water and the solvent was removed. The residue was purified by silica gel chromatography using 48% ethyl acetate, 48% hexane, and 4% methanol resulting in 2.0 g of an oil.

WORKUP

后处理

  1. additionTo a flask were added 0.6 g
  2. stirringAfter stirring for 1 hour
  3. extractionthe product was extracted with 60 ml of 50% ethyl acetate, 50% hexane
  4. washThe organic layer was washed with 30 ml water
  5. customthe solvent was removed
  6. customThe residue was purified by silica gel chromatography