HRID482078
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
3-Benzyloxyphenyl acetate (4.84 g, 20 mmol), as prepared in the preceding step, in tetrahydrofuran (50 mL) was treated with 1N NaOH (30 mL) for 3 h at room temperature. The mixture was acidified with 1N HCl and extracted into ethyl acetate (3×100 ML). The organic phase was washed with brine (2×50 mL), dried over Na2SO4, and concentrated in vacuo. The residue was then purified by flash column chromatography (methylene chloride) to give the title compound as a colorless liquid (3.80 g, 96%). 1H-NMR (300 MHz, CDCl3) δ 5.01 (s, 2H), 5.09 (s, 1fH), 6.47 (m, 2H), 6.56 (dd, 1H), 7.11 (t, 1H), 7.39 (m, 5H).
WORKUP
后处理
- extractionextracted into ethyl acetate (3×100 ML)
- washThe organic phase was washed with brine (2×50 mL)
- dry with materialdried over Na2SO4
- concentrationconcentrated in vacuo
- customThe residue was then purified by flash column chromatography (methylene chloride)