Ethanol → 3-Phenoxybutan-2-one oxime

HRID 1288235

반응식

HRID 1288235 반응식
[O:1]([CH:8]([CH3:12])[C:9](=O)[CH3:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C(O)C.Cl.[NH2:17][OH:18]>O>[O:1]([CH:8]([CH3:12])[C:9](=[N:17][OH:18])[CH3:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

참가 물질

5

반응물 3

HCID 702EthanolHCID 443297Hydroxyamine hydrochlorideHCID 27644743-Phenoxy-2-butanone

생성물 1

HCID 867340893-Phenoxybutan-2-one oxime

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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°.

후처리

  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°)

출처 및 근거

ORD 기록
ord-109a364803a944dbae0328df6d223e6f
출처 데이터셋
uspto-grants-1976_10
특허 번호
US03987158

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