Sodium Bicarbonate → HCID 178432730, Verbindung

HRID 216318

Reaktionsgleichung

Reaktionsgleichung von HRID 216318
[CH3:1][C:2]([CH3:12])([CH3:11])[CH2:3][C:4]1[N:5]=[C:6]([CH3:10])[N:7](O)[CH:8]=1.C(=O)(O)[O-].[Na+]>CO.[Cl-].[Ti+3].[Cl-].[Cl-]>[CH3:1][C:2]([CH3:12])([CH3:11])[CH2:3][C:4]1[N:5]=[C:6]([CH3:10])[NH:7][CH:8]=1

Komponenten

5

Edukt 2

HCID 516892Sodium BicarbonateHCID 686676414-(2,2-dimethylpropyl)-2-methyl-1H-imidazol-1-ol

Produkt 1

HCID 178432730HCID 178432730, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 10313229titanium(III) trichlorideKatalysatorHCID 887MethanolLösungsmittel

Versuchsvorschrift

Titanium (III) chloride (30% weight solution in 2N HCl) (600 mL, 1.5 mol) was added to an ambient temperature solution of 4-(2,2-dimethylpropyl)-2-methyl-1H-imidazol-1-ol (ca. 0.56 mmol) in methanol (1200 mL). After stirring at ambient temperature for a few days, the reaction mixture was basified with saturated aqueous sodium bicarbonate until the black solution turned white. The reaction mixture was extracted with ether. The combined organic extracts were washed with brine, dried (magnesium sulfate), filtered and concentrated in vacuo. Chromatography over silica eluting with 10-20% ethyl acetate/hexane afforded 4-(2,2-dimethylpropyl)-2-methyl-1H-imidazole.

Aufarbeitung

  1. extractionThe reaction mixture was extracted with ether
  2. washThe combined organic extracts were washed with brine
  3. dry with materialdried (magnesium sulfate)
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-322421c136d749628ace9adadd934aeb
Quelldatensatz
uspto-grants-2012_06
Patentnummer
US08193228B2

Verknüpfte Notizen

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