HRID1196953
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A solution of 2-chloro-2',4'-difluoroacetophenone (19.0 g) and anhydrous sodium acetate (16.4 g) in acetic acid (50 ml) was heated under reflux for 4 hours and then evaporated. The residue was partitioned between ethyl acetate and water. The organic layer was separated, washed with sodium bicarbonate solution and dried (Na2SO4). Evaporation of the solvent gave an oil which was triturated with hexane. The resulting solid was filtered off, washed with hexane and dried to give the title compound, (16.2 g), m.p. 54°-56°.
WORKUP
后处理
- temperatureunder reflux for 4 hours
- customevaporated
- customThe residue was partitioned between ethyl acetate and water
- customThe organic layer was separated
- washwashed with sodium bicarbonate solution
- dry with materialdried (Na2SO4)
- customEvaporation of the solvent
- customgave an oil which
- customwas triturated with hexane
- filtrationThe resulting solid was filtered off
- washwashed with hexane
- customdried