Reaktion #2295091

ord-a6b4d9eb1f4e4cedace107636b0caf47

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Filtrationfiltered
  2. 2
    Sonstigeto obtain a yellow filtrate
  3. 3
    EinengenThe filtrate was concentrated under reduced pressure
  4. 4
    SonstigeThe resulting residue was purified by silica gel column chromatography (eluent: n-hexane)

Vorschrift

[5-(5-Bromo-thiophen-2-yl)-1-(2,4-difluoro-phenyl)-4,5-dihydro-1H-pyrazol-3-yl]-methanol (12.9 g, 34.5 mmol) prepared in Step 4 and magnesium dioxide (MnO2) (30.0 g, 344.6 mmol) were added to dichloromethane (115.0 mL). The reaction mixture was stirred at room temperature for 3 days and then filtered to obtain a yellow filtrate. The filtrate was concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography (eluent: n-hexane) to give 9.1 g of the titled compound as a yellow liquid.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09376420B2uspto-grants-2016_06