Reaktion #163209

ord-4d3a8d87c2894a01abf4a777a2990f2a

Lösungsmittel

Reaktionsbedingungen

Temperatur
60°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe mixture is then subjected to HPLC purification

Vorschrift

To a solution of (4-{4-[2-(3-fluorophenylamino)-pyrimidin-5-yl]-phenyl}-cyclohexyl)-acetic acid methyl ester (crude from above) in DMF (2.5 mL) is added LiOH (10% solution, 1 mL) and the reaction mixture is heated at 60° C. for 1.5 h. The mixture is then subjected to HPLC purification to give the title compound: 1H NMR (400 MHz, DMSO-d6) δ 1.09-1.15 (m, 1H) 1.50 (td, J=12.44, 9.98 Hz, 1H) 1.63 (d, J=5.31 Hz, 6H) 2.37 (d, J=7.58 Hz, 2H) 6.76 (td, J=8.21, 2.27 Hz, 1H) 7.28-7.39 (m, 4H) 7.52 (dd, J=8.34, 1.26 Hz, 1H) 7.65 (s, 1H) 7.63 (t, J=4.04 Hz, 2H) 7.87 (d, J=12.38 Hz, 1H) 8.84-8.86 (m, 2H) 9.99 (s, 1H); (M+H)+=406.2.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08835451B2uspto-grants-2014_09