HRID2307534
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
To a solution of 19.71 g (0.18 mol) of 2-acetylfuran in 120 ml of methylene chloride were added 42.9 ml (2.0 eq) of 4-fluorobenzylchloride and 36.6 g (1.5 eq) of zinc chloride. The mixture was refluxed for 12 hours. The precipitated crystal was filtered and washed with methylene chloride. The obtained solid was dissolved in water and extracted with ethylacetate. The organic layer was washed with water and a diluted aqueous solution of sodium hydrogencarbonate and dried over sodium sulfate. The solvent was evaporated under reduced pressure. The residue was recrystallized from n-hexane to give 16.4 g of 2-acetyl-5-(4-fluorobenzyl)furan. Yield: 42%. Mp: 27-29° C.
WORKUP
后处理
- temperatureThe mixture was refluxed for 12 hours
- filtrationThe precipitated crystal was filtered
- washwashed with methylene chloride
- dissolutionThe obtained solid was dissolved in water
- extractionextracted with ethylacetate
- washThe organic layer was washed with water
- dry with materiala diluted aqueous solution of sodium hydrogencarbonate and dried over sodium sulfate
- customThe solvent was evaporated under reduced pressure
- customThe residue was recrystallized from n-hexane