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

HRID 1742541ノート

反応式

HRID 1742541 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 ml 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-2butenoyl)isoxazole was obtained as colorless oil. Analytical results of the crystals obtained: Yield: 3.6 g (67%).

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-ee1018622db04ba3bc27d027400064c5
出典データセット
uspto-grants-1994_08
特許番号
US05338857

反応ノート

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