HRID1386084
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
A mixture of 2,3-diamino-5-fluoropyridine (0.3 g, 2.4 mmol) and 3-bromo-2-butanon (0.36 g, 2.4 mmol) in ethanol (20 ml) was refluxed for 10 h. The solvent was evaporated under reduced pressure. The residue was dissolved in methylene chloride and was treated with a bicarbonate solution. The organic layer was separated, dried over sodium sulfate and evaporated under reduced pressure. The residue was purified with column chromatography on silica gel with methanol:methylene chloride (1:20) as eluent to give 0.16 g (37%) of the title compound.
WORKUP
后处理
- temperaturewas refluxed for 10 h
- customThe solvent was evaporated under reduced pressure
- dissolutionThe residue was dissolved in methylene chloride
- additionwas treated with a bicarbonate solution
- customThe organic layer was separated
- dry with materialdried over sodium sulfate
- customevaporated under reduced pressure
- customThe residue was purified with column chromatography on silica gel with methanol:methylene chloride (1:20) as eluent