反応 #91378

ord-a62da2b091d0470baad433db2f5db95c

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他The titled compound was synthesized
  2. 2
    その他The product was purified by column chromatography
  3. 3
    洗浄eluting with mixture of chloroform/ethanol/20% water solution of ammonia (200:10:1)
  4. 4
    洗浄the final product was washed with diethyl ether

実験手順

The titled compound was synthesized according to the general procedure described for preparation of N4-cyclohexyl-5,6-dimethyl-N2-(pyridin-2-ylmethyl)pyrimidine-2,4-diamine (Example 1) using (4-fluorobenzyl)amine instead of (pyridin-2-ylmethyl)amine. The product 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 1.03-1.10 (m, 1H), 1.20-1.34 (m, 2H), 1.59 (s, 1H), 1.68 (t, J=12.22 Hz, 4H), 1.87 (s, 3H), 2.23 (s, 3H), 3.86 (d, J=8.87 Hz, 1H), 4.52 (d, J=5.37 Hz, 2H), 7.14 (t, J=8.60 Hz, 2H), 7.33-7.38 (m, 2H), 7.57 (d, J=7.52 Hz, 1H), 8.10 (s, 1H), 12.78 (bs, 1H); MS (ESI) m/z 329.2 (M+1)+.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US09447051B2uspto-grants-2016_09