2-Methyl-2-butene → HCID 178524893, Verbindung

HRID 1424928

Reaktionsgleichung

Reaktionsgleichung von HRID 1424928
[OH2:1].O.P([O-])(O)(O)=O.[Na+].CC(=CC)C.Cl([O-])=O.[Na+].[F:18][C:19]([F:28])([F:27])[C:20]1[N:21]=[C:22]([CH:25]=[O:26])[NH:23][CH:24]=1>C(O)(C)(C)C>[F:28][C:19]([F:18])([F:27])[C:20]1[N:21]=[C:22]([C:25]([OH:1])=[O:26])[NH:23][CH:24]=1

Komponenten

6

Edukt 4

HCID 105532-Methyl-2-buteneHCID 23668197Sodium ChloriteHCID 23673460Sodium Phosphate, Monobasic, DihydrateHCID 178519985HCID 178519985, Verbindung

Produkt 1

HCID 178524893HCID 178524893, VerbindungAusbeute 98 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6386tert-ButanolLösungsmittel

Versuchsvorschrift

Sodium dihydrogenphosphate dihydrate (720 mg, 4.62 mmol), 2-methyl-2-butene (1.2 ml, 11.4 mmol) and sodium chlorite (420 mg, 4.64 mmol) were added under ice-cooling to a solution of 4-(trifluoromethyl)-1H-imidazole-2-carbaldehyde obtained in Example (33b) (375 mg, 2.29 mmol) in t-butyl alcohol (12 ml)/distilled water (5 ml), followed by stirring for 1.5 hours. The reaction solution was concentrated under reduced pressure, and then the residue was purified by reverse phase silica gel column chromatography (elution solvent: distilled water) to obtain 0.402 g of the title compound as a white solid (98%).

Aufarbeitung

  1. distillation)/distilled water (5 ml)
  2. concentrationThe reaction solution was concentrated under reduced pressure
  3. distillationthe residue was purified by reverse phase silica gel column chromatography (elution solvent: distilled water)

Quellen und Nachweise

ORD-Eintrag
ord-7476cebbffc243caba2845ee7fdefc84
Quelldatensatz
uspto-grants-2015_01
Patentnummer
US08927588B2

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