Chromic Acid → 5-Propionyl-3-phenylisoxazole

HRID 1450638

反応式

HRID 1450638 の反応式
[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]

参加物

5

反応物 2

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

生成物 1

HCID 151807665-Propionyl-3-phenylisoxazole

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒2 回HCID 962Water溶媒

反応条件

温度
60 °C

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-1f78464da91a4d619699984b4121eec8
出典データセット
uspto-grants-1997_02
特許番号
US05602160

関連ノート

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