Reaktion #91408

ord-b893dc03463344a1bf88d4a04a2f5e15

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 2-methylcyclohexanamine 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 (400 MHz, CDCl3) δ ppm 0.93 (bs, 3H), 1.28-1.42 (m, 6H), 1.62-1.70 (m, 1H), 1.78-1.89 (m, 2H), 1.93 (s, 3H), 2.07 (s, 3H), 2.95-3.04 (m, 1H), 4.43 (bs, 2H), 7.22 (t, J=7.30 Hz, 1H), 7.56 (d, J=7.76 Hz, 1H), 7.68-7.75 (m, 1H), 8.65 (d, J=4.92 Hz, 1H); MS (ESI) m/z 326.4.0 (M+1)+.

Quelle

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