HRID505776

反应详情

EQUATION

反应方程式

HRID 505776 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureThe reaction mixture was heated
  2. temperatureto reflux
  3. additionwas added
  4. additionwas added
  5. temperatureThe reaction was heated
  6. temperatureto reflux for 40 h
  7. temperatureAfter cooling down
  8. customevaporation of the solvent
  9. customgave a residue that
  10. customwas purified by flash chromatography on silica gel (1:9 AcOEt/petroleum ether)