Reaktion #91418

ord-4529210e7ba34ac1ae125d2de38b3487

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe titled compound was synthesized
  2. 2
    SonstigeThe crude material was purified by column chromatography
  3. 3
    Wascheneluting with mixture of chloroform/ethanol/20% water solution of ammonia (200:10:1)
  4. 4
    Waschenthe final product was washed with diethyl ether

Vorschrift

The titled compound was synthesized according to the procedure described for preparation of N4-cyclopentyl-5,6-dimethyl-N2-(pyridin-2-ylmethyl)pyrimidine-2,4-diamine (Example 29) using (4-fluorophenyl)amine instead of cyclopentanamine. The crude material was purified by column chromatography eluting with mixture of chloroform/ethanol/20% water solution of ammonia (200:10:1), and then the final product was washed with diethyl ether to afford the titled compound as a white solid. 1H NMR (300 MHz, CDCl3) δ ppm 2.07 (s, 3H), 2.34 (s, 3H), 4.69 (d, J=5.9 Hz, 2H), 5.98 (bs, 1H), 6.32 (s, 1H), 6.94 (t, J=8.3 Hz, 1H), 7.16 (t, J=7.5 Hz, 1H), 7.31 (d, J=7.6 Hz, 1H), 7.36-7.42 (m, 2H), 7.61 (t, J=7.5 Hz, 1H), 8.58 (d, J=5.4 Hz, 1H); MS (ESI) m/z 324.0 (M+1)+.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09447051B2uspto-grants-2016_09