HRID2073801

反应详情

EQUATION

反应方程式

HRID 2073801 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 2,3-diaminopyridine (1.09 g) in methanol (22 ml) was added 2-methyl-6-methoxycarbonylaminobenzyl chloride (2.14 g) and potassium carbonate (1.38 g) at room temperature and the mixture was stirred for 1.5 hours. The insoluble material was removed by filtration and methanol in the filtrate was evaporated under reduced pressure. The residue was subjected to column chromatography on silica gel (30 g) and eluted with a mixture of chloroform and methanol (100:1) to give a crystalline product. The crystals were triturated with diisopropyl ether to give 2-amino-3-(2-methyl-6-methoxycarbonylaminobenzylamino)pyridine (1.44 g).

WORKUP

后处理

  1. customThe insoluble material was removed by filtration and methanol in the filtrate
  2. customwas evaporated under reduced pressure
  3. washeluted with a mixture of chloroform and methanol (100:1)
  4. customto give a crystalline product
  5. customThe crystals were triturated with diisopropyl ether