HRID2095316

反应详情

EQUATION

反应方程式

HRID 2095316 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3-Fluoro-5-iodobenzaldehyde, monomethyl malonate, and a catalytic amount of pyrrolidine are heated in pyridine. After cooling, the solvent is distilled off in vacuo. 2N HCl and ethyl acetate are added to the residue, and the phases are separated. The organic layer is washed with brine and dried over Na2SO4. After evaporation, the residue is purified by CC on silica gel with EtOAc/hexane. Evaporation of appropriate fractions yields the title compound.

WORKUP

后处理

  1. temperatureAfter cooling
  2. distillationthe solvent is distilled off in vacuo
  3. addition2N HCl and ethyl acetate are added to the residue
  4. customthe phases are separated
  5. washThe organic layer is washed with brine
  6. dry with materialdried over Na2SO4
  7. customAfter evaporation
  8. customthe residue is purified by CC on silica gel with EtOAc/hexane
  9. customEvaporation of appropriate fractions