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Methanol → Methyl 4-bromooxazole-5-carboxylate

HRID 1157966
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1157966
[Br:1][C:2]1[N:3]=[C:4]([Si](C(C)C)(C(C)C)C(C)C)[O:5][C:6]=1[CH:7]=[O:8].[C-]#N.[Na+].[CH3:22][OH:23]>[O-2].[O-2].[Mn+4]>[CH3:22][O:23][C:7]([C:6]1[O:5][CH:4]=[N:3][C:2]=1[Br:1])=[O:8]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 887MethanolHCID 8929Sodium CyanideHCID 25232594HCID 25232594, Verbindung

Produkt 1

HCID 59511829Methyl 4-bromooxazole-5-carboxylate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 178418406HCID 178418406, VerbindungKatalysator

Versuchsvorschrift

To a mixture of 4-bromo-2-triisopropylsilanyloxazole-5-carboaldehyde (1.94 g) and methanol (40 mL) there were added sodium cyanide (1.43 g) and manganese dioxide (10.2 g) in that order, and the mixture was stirred overnight at room temperature. The mixture was filtered through Celite, the Celite was washed with ethyl acetate (200 mL), and the washed solution was combined with the filtrate. After sufficiently shaking the mixture, the organic layer was separated off and washed with a 1N aqueous sodium hydroxide solution (200 mL), and then dried over anhydrous magnesium sulfate. The mixture was filtered to obtain a filtrate, and the solvent in the filtrate was distilled off under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate-heptane mixture) to obtain the target compound (0.435 g) as a colorless solid.

Aufarbeitung

  1. filtrationThe mixture was filtered through Celite
  2. washthe Celite was washed with ethyl acetate (200 mL)
  3. stirringAfter sufficiently shaking the mixture
  4. customthe organic layer was separated off
  5. washwashed with a 1N aqueous sodium hydroxide solution (200 mL)
  6. dry with materialdried over anhydrous magnesium sulfate
  7. filtrationThe mixture was filtered
  8. customto obtain a filtrate
  9. distillationthe solvent in the filtrate was distilled off under reduced pressure
  10. customThe residue was purified by silica gel column chromatography (ethyl acetate-heptane mixture)

Quellen und Nachweise

ORD-Eintrag
ord-ffeb7e37d64940208dd36d1922e390d3
Quelldatensatz
uspto-grants-2010_10
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07807690B2

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