Reaktion #646330

ord-240680aa7fb44d5aa653925dcf4c5aa6

Lösungsmittel

Reaktionsbedingungen

Temperatur
45°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturto cool
  2. 2
    Sonstigepurified by flash chromatography, elution
  3. 3
    Filtrationthe product is filtered
  4. 4
    Waschenwashed with MeOH

Vorschrift

A solution containing 311 mg (0.56 mmol) of compound A 3-(2,4-dichlorophenyl)-1,9-dimethyl-6-{1-[2-(tetrahydropyran-2-yloxy)ethyl]-1H-pyrazol-3-yl}-1,9-dihydropyrido[2,3-b]indol-2-one, 2.7 ml of acetic acid, 1.3 ml of THF and 0.7 ml of H2O is heated at 45° C. for 16 h. The reaction medium is allowed to cool, adsorbed onto silica and purified by flash chromatography, elution being carried out with EtOAc/20% cyclohexane, then 100% EtOAc, and, finally, EtOAc/5% MeOH. The residue is taken up in MeOH and the product is filtered and then washed with MeOH.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08063061B2uspto-grants-2011_11