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
Over about 1 hour, a solution of 22 g of hydroxylamine hydrochloride and 26 g of anhydrous sodium acetate in 110 ml of water is added dropwise at room temperature to a solution of 64 g of 4-phenoxyphenoxyacetone in 260 ml of ethanol. After the slightly exothermic reaction has subsided, the mixture is stirred for a further 3.5 hours at reflux temperature. Subsequently, the ethanol is distilled off from the reaction mixture by rotary evaporation, the aqueous residue is extracted three times with a 2:1 mixture of ether and hexane, the combined organic phases are washed with water and with 10% sodium bicarbonate solution and then dried over sodium sulfate. The solvent is then distilled off. Recrystallisation from a mixture of diethyl ether and pentane affords 4-phenoxyphenoxyacetone oxime with a melting point of 59°-61° C.
WORKUP
后处理
- customAfter the slightly exothermic reaction
- temperatureat reflux temperature
- distillationSubsequently, the ethanol is distilled off from the reaction mixture by rotary evaporation
- extractionthe aqueous residue is extracted three times
- additionwith a 2:1 mixture of ether and hexane
- washthe combined organic phases are washed with water and with 10% sodium bicarbonate solution
- dry with materialdried over sodium sulfate
- distillationThe solvent is then distilled off
- customRecrystallisation
- additionfrom a mixture of diethyl ether and pentane