HRID638935
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
- 0 °C
PROCEDURE
实验过程
To a stirred solution of 3,4-dimethoxy-5-(trimethylsilanylethynyl)benzoic acid (5.56 g, 20 mmol) in THF (115 mL) at 0° C. was added TBAF (1.0 M solution in THF, 30 mL, 30 mmol). The resulting solution was stirred at 0° C. for 30 min, then the reaction mixture was diluted with 1 N HCl aqueous solution (200 mL), extracted with EtOAc (3×70 mL). The combined organic layer was washed with brine (100 mL), dried over Na2SO4, concentrated in vacuo to give 3-ethynyl-4,5-dimethoxybenzoic acid (4.0 g). The product was used without further purification.
WORKUP
后处理
- extractionextracted with EtOAc (3×70 mL)
- washThe combined organic layer was washed with brine (100 mL)
- dry with materialdried over Na2SO4
- concentrationconcentrated in vacuo