Reaktion #91412

ord-9bff60c1848e45e9a6959fdfdef87ad2

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 (cyclopentylmethyl)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, DMSO-d6) δ ppm 1.00-1.09 (m, 2H), 1.30-1.38 (m, 2H), 1.38-1.49 (m, 4H), 1.80-1.94 (m, 4H), 2.26 (s, 3H), 3.14 (bs, 2H), 4.70 (bs, 2H), 7.37-7.42 (m, 2H), 7.91 (t, J=7.52, 1H), 8.09-8.13 (m, 1H), 8.43 (s, 1H), 8.55-8.62 (m, 1H), 12.65 (bs, 1H); MS (ESI) m/z 312.8 (M+1)+.

Quelle

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