Reaktion #71737

ord-dfb5dbc140d94e42ae20fad4d81cbb8b

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

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

Vorschrift

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%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08536197B2uspto-grants-2013_09