HRID1181125
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
A 50 mL round bottomed flask was charged with 3-[2-bromomethyl-4-(tert-butyldiphenylsilanyloxy)phenyl]propionic acid tert-butyl ester (1.0 g, 1.81 mmol), anhydrous DMF (10 mL), and then 4-trifluoromethylphenol (0.44 g, 2.7 mmol) and cesium carbonate (0.88 g, 2.7 mmol). The reaction mixture was stirred at ambient temperature under a nitrogen atmosphere for 18 h and concentrated. The residue was diluted with EtOAc (100 mL). The organic layer was washed with brine (2×), dried (Na2SO4), and concentrated to a yellow oil. The crude residue was purified using radial (EtOAc:hexanes 15:85 to 50:50) to give a yellow oil (0.66 g, 58%). MS (ES) m/e 635 (M+1).
WORKUP
后处理
- concentrationconcentrated
- additionThe residue was diluted with EtOAc (100 mL)
- washThe organic layer was washed with brine (2×)
- dry with materialdried (Na2SO4)
- concentrationconcentrated to a yellow oil
- customThe crude residue was purified