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
CONDITIONS
反应条件
- 温度
- 27.5 °C
PROCEDURE
实验过程
Ethyl bromopyruvate (2.15 g, 11.04 mmol) was added to stirred solution of 2-aminopyrazine (1 g, 10.5 mmol) in 1,2-Dimethoxy ethane (10 mL). The reaction mixture was stirred at 20-35° C. for 2 h. The mixture was then filtered to obtain a solid precipitate which was dried well, dissolved in EtOH (10 mL) and refluxed for 2 h. This mixture was concentrated, diluted with aqueous saturated sodium bicarbonate solution, extracted with chloroform. The chloroform layer was washed with water followed by brine solution, dried over anhydrous sodium sulphate and concentrated under reduced pressure to afford the crude product, which was purified by column chromatography (using 60-120 silica gel and 60% EtOAc in Hexane as eluent) to afford 450 mg of the title compound.
WORKUP
后处理
- filtrationThe mixture was then filtered
- customto obtain a solid precipitate which
- customwas dried well
- dissolutiondissolved in EtOH (10 mL)
- temperaturerefluxed for 2 h
- concentrationThis mixture was concentrated
- additiondiluted with aqueous saturated sodium bicarbonate solution
- extractionextracted with chloroform
- washThe chloroform layer was washed with water
- dry with materialdried over anhydrous sodium sulphate
- concentrationconcentrated under reduced pressure
- customto afford the crude product, which
- customwas purified by column chromatography (using 60-120 silica gel and 60% EtOAc in Hexane as eluent)