Reaktion #1129459

ord-61cf1a7a73304f0795512eed9f23518f

Lösungsmittel

Reaktionsbedingungen

Temperatur
70°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe TFA was removed in vacuo and 2M NH3/MeOH
  2. 2
    workup.ADDITIONwas added
  3. 3
    Sonstigesolvent was removed in vacuo
  4. 4
    SonstigeThe product was purified by flash chromatography
  5. 5
    Wascheneluting with MeOH(NH3)/DCM (2-6%)

Vorschrift

A mixture of 4-(8-(3-(9-(4-methoxybenzyl)-9H-purin-6-yl)pyridin-2-ylamino)-7-methylquinazolin-4-ylamino)benzonitrile (91 mg, 154 μmol) in TFA (3 mL) was heated at 70° C. for 3 h. The TFA was removed in vacuo and 2M NH3/MeOH was added. The mixture was stirred for 5 min and solvent was removed in vacuo. The product was purified by flash chromatography eluting with MeOH(NH3)/DCM (2-6%) to give 4-(8-(3-(9H-purin-6-yl)pyridin-2-ylamino)-7-methylquinazolin-4-ylamino)benzonitrile. MS (ESI, pos. ion) m/z: 471.2 [M+H]+

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08557830B2uspto-grants-2013_10