Reaktion #167911

ord-ec4f98bd8a074ed3ad7c9945ae5d4810

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigethe solvent is evaporated off under reduced pressure
  2. 2
    Extraktionthe product is extracted with dichloromethane
  3. 3
    FiltrationThe organic phase is filtered on a hydrophobic cartridge
  4. 4
    Einengenconcentrated under reduced pressure
  5. 5
    SonstigeThe solid obtained
  6. 6
    Sonstigeis triturated with diisopropyl ether

Vorschrift

To a suspension of 0.76 g (1.67 mmol) of tert-butyl {4-[6-chloro-2-(4-chlorophenyl)imidazo[1,2-b]pyridazin-3-yl]pyrid-2-yl}carbamate in 8 mL of dichloromethane are added 4 mL (48 mmol) of hydrochloric acid. After stirring for 2 hours at room temperature, the solvent is evaporated off under reduced pressure, the oily residue is taken up with aqueous ammonia and the product is extracted with dichloromethane. The organic phase is filtered on a hydrophobic cartridge and concentrated under reduced pressure. The solid obtained is triturated with diisopropyl ether to give 0.56 g of solid after filtering off and drying under reduced pressure.

Quelle

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