HRID35279

反应详情

EQUATION

反应方程式

HRID 35279 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. customAfter the slightly exothermic reaction
  2. temperatureat reflux temperature
  3. distillationSubsequently, the ethanol is distilled off from the reaction mixture by rotary evaporation
  4. extractionthe aqueous residue is extracted three times
  5. additionwith a 2:1 mixture of ether and hexane
  6. washthe combined organic phases are washed with water and with 10% sodium bicarbonate solution
  7. dry with materialdried over sodium sulfate
  8. distillationThe solvent is then distilled off
  9. customRecrystallisation
  10. additionfrom a mixture of diethyl ether and pentane