HRID1398720
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
A mixture of gallic acid (4 g, 21.27 mmol), benzyl chloride (19.5 mL, 0.170 mol), tertiary butyl ammonium iodide (catalytic) and K2CO3 (14.67 g, 106 mmol) in acetone (50 mL) was refluxed for 6 h. The mixture was filtered and the filter cake was washed well with acetone. The combined filtrate and washing solvent were evaporated to dryness in vacuo. The residue was dissolved in ethyl acetate (50 mL), washed with H2O (20×2 mL) and brine (30 mL), dried over Na2SO4 and evaporated to dryness. The crude residue was purified by silica gel column chromatography using 5% ethyl acetate in hexane as eluent to obtain pure 1a as white solid (9.01 g, 80%).
WORKUP
后处理
- temperaturewas refluxed for 6 h
- filtrationThe mixture was filtered
- washthe filter cake was washed well with acetone
- washThe combined filtrate and washing solvent
- customwere evaporated to dryness in vacuo
- dissolutionThe residue was dissolved in ethyl acetate (50 mL)
- washwashed with H2O (20×2 mL) and brine (30 mL)
- dry with materialdried over Na2SO4
- customevaporated to dryness
- customThe crude residue was purified by silica gel column chromatography