HRID1181126
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 100 mL round bottomed flask was charged with 3-[4-(tert-butyldiphenylsilanyloxy)-2-(4-trifluoromethylphenoxymethyl)phenyl]propionic acid tert-butyl ester (0.65 g, 1.02 mmol), anhydrous THF (40 mL), and then tetrabutylammonium fluoride (3.1 mL, 3.1 mmol, 1.0 M in THF). The reaction was stirred under a nitrogen atmosphere for 1.5 h and was concentrated. The residue was diluted with EtOAc (100 mL). The organic layer was washed with brine (2×), dried (Na2SO4), and concentrated to an orange oil. The crude oil was purified using radial chromatography (EtOAc:hexanes 15:85) to give a white solid (0.31 g, 77%). MS (ES) m/e 395 (M−1).
WORKUP
后处理
- concentrationwas concentrated
- additionThe residue was diluted with EtOAc (100 mL)
- washThe organic layer was washed with brine (2×)
- dry with materialdried (Na2SO4)
- concentrationconcentrated to an orange oil
- customThe crude oil was purified