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
The title compound was prepared by stirring a mixture of 2,5-bis(2,2,2-trifluoroethoxy)acetophenone (200 mg, 0.633 mmol), 4-chlorobenzaldehyde (89 mg, 0.633 mmol), methanol (5 ml) and saturated NaOH (200 ul) at room temperature for 4 h. The mixture was diluted with ethyl acetate (100 ml), wash with water (50 ml) and saturated aqueous NaCl (50 ml), dried over anhydrous sodium sulfate and concentrated in vacuo. The residue was purified by column chromatography using hexane:ethyl acetate (5:1, 4:1) to give a yellow solid (143 mg, 51%). 1H NMR (CDCl3): 7.65 (d, J=15.9 Hz, 1H), 7.54 (d, J=8.4 Hz, 2H), 7.44 (d, J=15.9 Hz, 1H), 7.38 (d, J=8.4 Hz, 2H), 7.31 (d, J=3.3 Hz, 1H), 7.14 (dd, J=3.3, 9.3 Hz, 1H), 6.95 (d, J=9.0 Hz, 1H), 4.45-4.32 (m, 4H).
WORKUP
后处理
- washwash with water (50 ml) and saturated aqueous NaCl (50 ml)
- dry with materialdried over anhydrous sodium sulfate
- concentrationconcentrated in vacuo
- customThe residue was purified by column chromatography