HRID1243745
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
4-Chloro-2-fluorobenzonitrile (0.34 g, 2.2 mmol), 3-allyl-4-hydroxybenzaldehyde (0.34 g, 2.1 mmol) and potassium fluoride (6.37 g, 6.3 mmol) were heated with stirring in dry DMF (4 mL) at 120° C. for 4 h. The reaction mixture was cooled, poured into 0.1N sodium hydroxide solution and extracted with ethyl acetate. The ethyl acetate layer was separated, washed with 0.1N sodium hydroxide solution (3×), water (2×), brine (1×), and dried over MgSO4. After filtration, the solvent was removed in vacuo and the residue purified by chromatography to give 2-(2-allyl-4-formyl-phenoxy)4-chlorobenzonitrile (0.09 g, 15%) as a colourless oil.
WORKUP
后处理
- temperatureThe reaction mixture was cooled
- extractionextracted with ethyl acetate
- customThe ethyl acetate layer was separated
- washwashed with 0.1N sodium hydroxide solution (3×), water (2×), brine (1×)
- dry with materialdried over MgSO4
- filtrationAfter filtration
- customthe solvent was removed in vacuo
- customthe residue purified by chromatography