HRID2073801
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customThe insoluble material was removed by filtration and methanol in the filtrate
- customwas evaporated under reduced pressure
- washeluted with a mixture of chloroform and methanol (100:1)
- customto give a crystalline product
- customThe crystals were triturated with diisopropyl ether