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

HRID 1450653Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1450653
[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

Komponenten

5

Edukt 3

HCID 61680MAGNESIUM SILICATE (synthetic)HCID 2763417(3-Phenyl-5-isoxazolyl)methanolHCID 178418287HCID 178418287, Verbindung

Produkt 1

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

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

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.

Aufarbeitung

  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

Quellen und Nachweise

ORD-Eintrag
ord-ec2b2c4b1efa499986b47da6f3ed4496
Quelldatensatz
uspto-grants-1997_02
Patentnummer
US05602160

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