HRID1766081
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
5-Cyano-4-(3-methoxyphenyl)-2-methylthio-6-vinyl-pyrimidine (example 25a) was dissolved in a mixture of ethanol (2 ml) and toluene (2 ml). Potassium carbonate (690 mg) and diethylmalonate (272 μl) were added and the mixture was stirred at room temperature for 4 h. The reaction mixture was then poured in a mixture of 0.5M aq. HCl (25 ml) and EtOAc (50 ml). The organic layer was washed with H2O (50 ml) and sat. aq. NaCl (50 ml), dried (MgSO4) and concentrated under reduced pressure. The title compound was purified by chromatography on silica gel with toluene/EtOAC=100/0 to 95/5 (v/v) as eluent.
WORKUP
后处理
- washThe organic layer was washed with H2O (50 ml) and sat. aq. NaCl (50 ml)
- dry with materialdried (MgSO4)
- concentrationconcentrated under reduced pressure
- customThe title compound was purified by chromatography on silica gel with toluene/EtOAC=100/0 to 95/5 (v/v) as eluent