HRID591556
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
CONDITIONS
反应条件
- 温度
- 100 °C
PROCEDURE
实验过程
To a mixture of methyl(4-(((trifluoromethyl)sulfonyl)oxy)-6-((triisopropylsilyl)oxy)-1-benzothiophen-3-yl)acetate (5.8 g) and DMF (dry) (80 mL) were added zinc cyanide (2.095 mL) and Pd(Ph3P)4 (1.273 g) at room temperature, and the mixture was stirred at 100° C. for 20 h. The mixture was cooled to room temperature. The mixture was poured into water at room temperature and extracted with EtOAc. The organic layer was separated, washed successively with water and brine, dried over MgSO4 and concentrated in vacuo. The residue was purified by silica gel column chromatography (EtOAc/hexane) to give the title compound (1.920 g).
WORKUP
后处理
- temperatureThe mixture was cooled to room temperature
- extractionextracted with EtOAc
- customThe organic layer was separated
- washwashed successively with water and brine
- dry with materialdried over MgSO4
- concentrationconcentrated in vacuo
- customThe residue was purified by silica gel column chromatography (EtOAc/hexane)