HRID427502
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
Ethyl 5,6-diaminonicotinate (1.4 g, 7.7 mmol) and 3-bromo-2-butanon (1.16 g, 7.2 mmol) were added to 1,2-dimethoxyethan (50 ml) and refluxed for 20 h. The solvent was evaporated under reduced pressure and the residue was dissolved in methylene chloride. The methylene chloride solution was washed with saturated sodium bicarbonate and dried (Na2SO4). The solvent was evaporated under reduced pressure and the residue was purified by column chromatography on silica gel using methylene chloride:methanol (10:1) as eluent to give 0.3 g (17%) of the title compound.
WORKUP
后处理
- temperaturerefluxed for 20 h
- customThe solvent was evaporated under reduced pressure
- dissolutionthe residue was dissolved in methylene chloride
- washThe methylene chloride solution was washed with saturated sodium bicarbonate
- dry with materialdried (Na2SO4)
- customThe solvent was evaporated under reduced pressure
- customthe residue was purified by column chromatography on silica gel