MAGNESIUM SILICATE (synthetic) → 3-Phenyl-1,2-oxazole-5-carbaldehyde

HRID 1742535ノート

反応式

HRID 1742535 の反応式
[C:1]1([C:7]2[CH:11]=[C:10]([CH2:12][OH:13])[O:9][N:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[O-][Si]([O-])=O.[Mg+2].[Cr](Cl)([O-])(=O)=O.[NH+]1C=CC=CC=1>ClCCl>[C:1]1([C:7]2[CH:11]=[C:10]([CH:12]=[O:13])[O:9][N:8]=2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

参加物

5

反応物 3

HCID 61680MAGNESIUM SILICATE (synthetic)HCID 2763417(3-Phenyl-5-isoxazolyl)methanolHCID 178418287HCID 178418287、化合物

生成物 1

HCID 113672673-Phenyl-1,2-oxazole-5-carbaldehyde

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

Dissolved in 500 ml of dichloromethane were 29 g (165.7 mmol) of 3-phenyl-5-hydroxymethylisoxazole prepared in Example 28 and 80 g of "Florisil" (trade mark), followed by the addition of 74 g (342.6 mmol) of pyridinium chlorochromate. They were reacted for 7 hours at room temperature. After an insoluble material was filtered off, the filtrate was added into water and then extracted with dichloromethane. After the solvent was distilled off, the residue was purified by silica gel chromatography (eluent: chloroform) so that 3-phenylisoxazole-5-aldehyde was obtained as crystals. Analytical results of the crystals obtained: Yield: 26.0 g (90.7%). Melting point: 67°-69° C.

後処理

  1. customThey were reacted for 7 hours at room temperature
  2. filtrationAfter an insoluble material was filtered off
  3. additionthe filtrate was added into water
  4. extractionextracted with dichloromethane
  5. distillationAfter the solvent was distilled off
  6. customthe residue was purified by silica gel chromatography (eluent: chloroform) so that 3-phenylisoxazole-5-aldehyde
  7. customwas obtained as crystals
  8. customAnalytical results of the crystals
  9. customobtained

出典と根拠

ORDレコード
ord-f5117cf7445a4a849d1c1e8cb6e34956
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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