HRID1288235
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
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
- temperatureThe resulting solution was refluxed for 31/2 hours
- customevaporated
- customThe residue was partitioned between water and ether
- extractionThe ether extract
- washwas washed with water
- dry with materialdried over anhydrous potassium carbonate
- customevaporated
- distillationThe residue was distilled
- customto give a fraction, b.p. 154°-155°/14 mm
- customwhich crystallised
- customRecrystallisation from petroleum ether (b.p. 60°-80°)