Reaktion #1112818

ord-b1d4b36f00c648308f9b3ee4936a52ad

Lösungsmittel

Reaktionsbedingungen

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

Aufarbeitung

  1. 1
    Sonstigeto give a colorless solution
  2. 2
    SonstigeThe crude reaction mixture
  3. 3
    Einengenwas concentrated in vacuo
  4. 4
    SonstigePurification by HPLC

Vorschrift

In a 25 mL round-bottomed flask, 6-bromo-1-(3-(6-tert-butyl-8-fluoro-1-oxophthalazin-2(1H)-yl)-2-(hydroxymethyl)phenyl)-1H-pyrrolo[2,3-b]pyridine-3-carbonitrile (14 mg, 25.6 μmol) and [hydrogen bis(dimethylphosphinito-kP)]platinum (II) (110 μg, 0.256 μmol, Eq: 0.01) were combined with Ethanol (2.99 ml) and Water (2.99 ml) to give a colorless solution. The reaction mixture was heated to 45° C. and stirred for 1 h. The crude reaction mixture was concentrated in vacuo. Purification by HPLC gave 6-bromo-1-[3-(6-tert-butyl-8-fluoro-1-oxo-1H-phthalazin-2-yl)-2-hydroxymethyl-phenyl]-1H-pyrrolo[2,3-b]pyridine-3-carboxylic acid amide (11 mg, 77%, [M+H]+ 565).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08729078B2uspto-grants-2014_05