Reaktion #5439

ord-d740cb40c09548b39dbf951d10f89106

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturthe mixture is heated
  2. 2
    Sonstigethe solvent is then evaporated under reduced pressure
  3. 3
    SonstigeThe crude product is purified by chromatography on a silica gel column (eluent: dichloromethane/methanol, 98/2 to 85/15) in order

Vorschrift

2.3 g (4.9 mmol) of 1-[2-[[2-[4-(5-chloro-2-methoxyphenyl)piperazin-1-yl]ethyl]amino]pyrimidin-4-ylcarbonyl]piperidin-4-amine, and 0.9 g (6.3 mmols) of 2-methylthiopyrimidin-4(1H)-one in solution in 40 ml of m-xylene are introduced into a 0.5 l, round bottomed flask and the mixture is heated at reflux of the m-xylene for 14 hours. The reaction mixture is cooled to room temperature and the solvent is then evaporated under reduced pressure. The crude product is purified by chromatography on a silica gel column (eluent: dichloromethane/methanol, 98/2 to 85/15) in order to obtain 1.56 g (2.74 mmols) of compound.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05244894uspto-grants-1993_09