Reaktion #1129470

ord-e4f7e095a28a48abaf665cfae76a65c9

Lösungsmittel

Reaktionsbedingungen

Temperatur
65°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeTFA was removed under vacuum
  2. 2
    workup.ADDITIONMeOH (2N, NH3) (20 ml) was added
  3. 3
    Sonstigesolvent was removed under vacuum
  4. 4
    SonstigeThe product was purified by flash chromatography
  5. 5
    Wascheneluting with MeOH/DCM (1-5%)

Vorschrift

A mixture of 4-(8-(3-(1-(4-methoxybenzyl)-1H-pyrazolo[3,4-d]pyrimidin-4-yl)pyridin-2-ylamino)-7-methylquinazolin-4-ylamino)benzonitrile (120 mg, 203 μmol) in TFA (3 ml) was heated at 65° C. for 3 hr. TFA was removed under vacuum. MeOH (2N, NH3) (20 ml) was added and then solvent was removed under vacuum. The product was purified by flash chromatography eluting with MeOH/DCM (1-5%) to give 4-(8-(3-(1H-pyrazolo[3,4-d]pyrimidin-4-yl)pyridin-2-ylamino)-7-methylquinazolin-4-ylamino)benzonitrile. MS (ESI pos. ion) m/z 471 (M+H+).

Quelle

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