HRID1288235

反应详情

EQUATION

反应方程式

HRID 1288235 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3-Phenoxybutan-2-one (69.6 g.) and ethanol (300 ml.) were added to a solution of hydroxylamine hydrochloride (70 g.) and fused sodium acetate (70 g.) in water (130 ml.). The resulting solution was refluxed for 31/2 hours and evaporated to near dryness under reduced pressure. The residue was partitioned between water and ether. The ether extract was washed with water, dried over anhydrous potassium carbonate and evaporated. The residue was distilled to give a fraction, b.p. 154°-155°/14 mm. which crystallised. Recrystallisation from petroleum ether (b.p. 60°-80°) gave pure 3-phenoxybutan-2-one oxime, m.p. 65°-67°.

WORKUP

后处理

  1. temperatureThe resulting solution was refluxed for 31/2 hours
  2. customevaporated
  3. customThe residue was partitioned between water and ether
  4. extractionThe ether extract
  5. washwas washed with water
  6. dry with materialdried over anhydrous potassium carbonate
  7. customevaporated
  8. distillationThe residue was distilled
  9. customto give a fraction, b.p. 154°-155°/14 mm
  10. customwhich crystallised
  11. customRecrystallisation from petroleum ether (b.p. 60°-80°)