HRID2095316
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
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
- temperatureAfter cooling
- distillationthe solvent is distilled off in vacuo
- addition2N HCl and ethyl acetate are added to the residue
- customthe phases are separated
- washThe organic layer is washed with brine
- dry with materialdried over Na2SO4
- customAfter evaporation
- customthe residue is purified by CC on silica gel with EtOAc/hexane
- customEvaporation of appropriate fractions