Reaktion #44139

ord-67d476a8c0ad4fd7bd9296396c7ef53d

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Wascheneluted with methanol
  2. 2
    EinengenThe basic fractions were concentrated under vacuum
  3. 3
    Sonstigepurified by column chromatography (SPE cartridge, Silica)

Vorschrift

To a stirred solution of 1-(3-{2-[4-(2-methyl-5-quinolinyl)-1-piperazinyl]ethyl}phenyl)-2-imidazolidinone (E85) in THF was added methyl iodide (1 eq.), followed by sodium hydride (1.2 eq), and the reaction was stirred for 60 minutes. The mixture was loaded onto an ion-exchange cartridge (SCX-2) and eluted with methanol followed by ammonia in methanol (1M). The basic fractions were concentrated under vacuum and purified by column chromatography (SPE cartridge, Silica) using as eluent a gradient from DCM-methanol (99:1) to DCM-methanol (98:2) affording the final compound (45% yield).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07732600B2uspto-grants-2010_06