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
CONDITIONS
反应条件
- 温度
- 85 °C
PROCEDURE
实验过程
To 258 g (0.94 mol) of a 50% aqueous solution of zinc chloride were added 69.3 g of water, 99.0 g (0.90 mol) of 2-acetylfuran and 260 g (1.80 mol) of 4-fluorobenzylchloride. The mixture was stirred at 85° C. for 6 hours. The reaction mixture was cooled and extracted with ethylacetate. The extract was washed with 1N hydrochloric acid, washed with an aqueous sodium hydrogencarbonate solution and removed under reduced pressure. The obtained residue was distilled under reduced pressure to give 145.4 g of crude 2-acetyl-5-(4-fluorobenzyl)furan (106-121° C./0.4 mmHg). The crude product was recrystallized from isopropylalcohol/n-hexane to give 84.4 g of 2-acetyl-5-(4-fluorobenzyl)furan. Yield: 43%.
WORKUP
后处理
- temperatureThe reaction mixture was cooled
- extractionextracted with ethylacetate
- washThe extract was washed with 1N hydrochloric acid
- washwashed with an aqueous sodium hydrogencarbonate solution
- customremoved under reduced pressure
- distillationThe obtained residue was distilled under reduced pressure