HRID591557
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
To a mixture of methyl(4-cyano-6-((triisopropylsilyl)oxy)-1-benzothiophen-3-yl)acetate (1.92 g) and EtOH (30 mL) was added potassium fluoride dihydrate (0.448 g) at room temperature, and the mixture was refluxed for 30 min. The mixture was concentrated under reduced pressure. The residue was poured into water at room temperature and extracted with EtOAc. The organic layer was separated, washed successively with 0.1N HCl and brine, dried over MgSO4 and concentrated in vacuo. The residue was crystallized from EtOAc-hexane to give the title compound (0.935 g).
WORKUP
后处理
- temperaturethe mixture was refluxed for 30 min
- concentrationThe mixture was concentrated under reduced pressure
- additionThe residue was poured into water at room temperature
- extractionextracted with EtOAc
- customThe organic layer was separated
- washwashed successively with 0.1N HCl and brine
- dry with materialdried over MgSO4
- concentrationconcentrated in vacuo
- customThe residue was crystallized from EtOAc-hexane