HRID505776
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 solution (0.33 M) of methyl 5-methyl-4-nitrothiophene-2-carboxylate in MeOH, was treated with benzaldehyde (1.5 eq.). The reaction mixture was heated to reflux and when it became a clear solution a catalytic amount of pyrrolidine (0.01 eq.) was added. After 18 h at reflux additional pyrrolidine (0.01 eq.) was added. The reaction was heated to reflux for 40 h. After cooling down, evaporation of the solvent gave a residue that was purified by flash chromatography on silica gel (1:9 AcOEt/petroleum ether) to afford the title compound (67%) as a solid.
WORKUP
后处理
- temperatureThe reaction mixture was heated
- temperatureto reflux
- additionwas added
- additionwas added
- temperatureThe reaction was heated
- temperatureto reflux for 40 h
- temperatureAfter cooling down
- customevaporation of the solvent
- customgave a residue that
- customwas purified by flash chromatography on silica gel (1:9 AcOEt/petroleum ether)