Reaktion #1891085

ord-d74563b07826453e8a6b0f5a747daba8

Lösungsmittel

Reaktionsbedingungen

Temperatur
155°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturAfter cooling
  2. 2
    Sonstigethe solvent is evaporated off under reduced pressure
  3. 3
    Sonstigethe residue is chromatographed on silica gel
  4. 4
    Wascheneluting with a mixture of dichloromethane and methanol (93:7)
  5. 5
    SonstigeThe product is then recrystallized from 40 mL of methanol

Vorschrift

A mixture of 4.03 g (13.1 mmol) of 6-chloro-2-phenyl-3-pyrid-4-ylimidazo[1,2-b]pyridazine and 4.4 g (29 mmol) of 4-pyrrolidin-1-ylpiperidine in 50 mL of ethanol is heated at 155° C. for 4 hours. After cooling, the solvent is evaporated off under reduced pressure and the residue is chromatographed on silica gel, eluting with a mixture of dichloromethane and methanol (93:7). The product is then recrystallized from 40 mL of methanol to give 1.5 g of yellow crystals after drying under reduced pressure.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08354405B2uspto-grants-2013_01