3-Phenyl-5-(1-hydroxy-2-methyl-2-butenyl)isoxazole → 3-Phenyl-5-(2-methyl-2-butenoyl)isoxazole

HRID 1450659ノート

反応式

HRID 1450659 の反応式
[C:1]1([C:7]2[CH:11]=[C:10]([CH:12]([OH:17])[C:13]([CH3:16])=[CH:14][CH3:15])[O:9][N:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1>C1C=CC=CC=1.[O-2].[O-2].[Mn+4]>[C:1]1([C:7]2[CH:11]=[C:10]([C:12](=[O:17])[C:13]([CH3:16])=[CH:14][CH3:15])[O:9][N:8]=2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

参加物

4

反応物 1

HCID 536910293-Phenyl-5-(1-hydroxy-2-methyl-2-butenyl)isoxazole

生成物 1

HCID 539504603-Phenyl-5-(2-methyl-2-butenoyl)isoxazole

試薬・触媒・溶媒 2

HCID 178418406HCID 178418406、化合物触媒HCID 241Benzene溶媒

実験手順

Dissolved in 100 m of benzene were 5.4 g (23.6 mmol) of 3 -phenyl-5-(1-hydroxy-2 -methyl-2 -butenyl)isoxazole, followed by the addition of 21.0 g (0.24 mol) of manganese dioxide. The mixture was stirred at room temperature for 24 hours. An insoluble material was filtered off and the solvent was distilled off under reduced pressure. The residue was purified by silica gel chromatography (eluent: 30:1 n-hexane/ethyl acetate), whereby 3-phenyl-5-(2-methyl-2-butenoyl)isoxazole was obtained as colorless oil.

後処理

  1. filtrationAn insoluble material was filtered off
  2. distillationthe solvent was distilled off under reduced pressure
  3. customThe residue was purified by silica gel chromatography (eluent: 30:1 n-hexane/ethyl acetate)

出典と根拠

ORDレコード
ord-8fadf0e05ca34cef9cbee07dd3d072ca
出典データセット
uspto-grants-1997_02
特許番号
US05602160

反応ノート

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