Reaktion #167914

ord-87a8fccc94de441592f1918692fa39bc

Lösungsmittel

Reaktionsbedingungen

Temperatur
135°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe solvent is then evaporated off under reduced pressure
  2. 2
    Sonstigethe oily residue is chromatographed on a column of silica gel
  3. 3
    Wascheneluting with a stepwise gradient of methanol and aqueous ammonia in dichloromethane (0/0/100 to 2/1/98)

Vorschrift

A mixture of 0.25 g (0.70 mmol) of 6-chloro-2-(4-fluorophenyl)-3-(2-methoxypyrid-4-yl)imidazo-[1,2-b]pyridazine and 0.37 g (2.8 mmol) of 2-(piperazin-1-yl)ethanol in 6 mL of pentanol is stirred at 135° C. for 18 hours. The solvent is then evaporated off under reduced pressure and the oily residue is chromatographed on a column of silica gel, eluting with a stepwise gradient of methanol and aqueous ammonia in dichloromethane (0/0/100 to 2/1/98). 0.136 g of product is isolated after trituration in diisopropyl ether, filtering off and drying under reduced pressure.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08846676B2uspto-grants-2014_09