Chromic Acid → 5-Propionyl-3-phenylisoxazole

HRID 1440317

반응식

HRID 1440317 반응식
[OH:1][CH:2]([C:5]1[O:9][N:8]=[C:7]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)[CH:6]=1)[CH2:3][CH3:4].[Cr](O)(O)(=O)=O>C(O)(=O)C.O>[C:2]([C:5]1[O:9][N:8]=[C:7]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)[CH:6]=1)(=[O:1])[CH2:3][CH3:4]

참가 물질

5

반응물 2

HCID 24425Chromic AcidHCID 151807655-(1-Hydroxypropyl)-3-phenylisoxazole

생성물 1

HCID 151807665-Propionyl-3-phenylisoxazole

시약·촉매·용매 2

HCID 176Acetic Acid용매2회HCID 962Water용매

반응 조건

온도
60 °C

실험 절차

In 130 ml of acetic acid, 19 g (93.6 mmol) of 5-(1-hydroxypropyl)-3-phenylisoxazole were dissolved. A solution which had been obtained by dissolving 6.4 g (64 mmol) of chromic acid in a mixed solution of 50 ml of acetic acid and 10 ml of water was added dropwise. The reaction mixture was heated at 60° C. for 3 hours and the solvent was distilled off under reduced pressure. The residue thus obtained was poured in ice water. Colorless crystals precipitated were collected by filtration and then dried under reduced pressure. The crystals were purified by chromatography on a silica gel (eluent: 2:8 hexane/chloroform), whereby 5-propionyl-3-phenylisoxazole was obtained as colorless crystals.

후처리

  1. customA solution which had been obtained
  2. additionwas added dropwise
  3. distillationthe solvent was distilled off under reduced pressure
  4. customThe residue thus obtained
  5. customColorless crystals precipitated
  6. filtrationwere collected by filtration
  7. customdried under reduced pressure
  8. customThe crystals were purified by chromatography on a silica gel (eluent: 2:8 hexane/chloroform)

출처 및 근거

ORD 기록
ord-05b34c996d434bc4bd2e65e2fef9c775
출처 데이터셋
uspto-grants-1996_03
특허 번호
US05498619

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