HRID1728887

反应详情

EQUATION

反应方程式

HRID 1728887 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To a 0° solution of 15 g of 2-(aminomethyl)pyridine, 15.44 g of triethylamine and 150 ml of methylene chloride is added 17.48 g of methanesulfonyl chloride in 100 ml of methylene chloride. The mixture is stirred at 0° C. for 1 hour followed by stirring at room temperature for 3 hours. The reaction is poured into saturated sodium bicarbonate and extracted with methylene chloride. The combined extracts are washed with saturated sodium chloride and concentrated in vacuo. The residue is purified by chromatography (silica gel: 10% methyl alcohol/ethyl acetate) to give 19.84 g of the desired product.

WORKUP

后处理

  1. stirringby stirring at room temperature for 3 hours
  2. extractionextracted with methylene chloride
  3. washThe combined extracts are washed with saturated sodium chloride
  4. concentrationconcentrated in vacuo
  5. customThe residue is purified by chromatography (silica gel: 10% methyl alcohol/ethyl acetate)