反应 #91453

ord-d0da03ab7c76452aadb9a618d66f85ff

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

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

实验过程

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 (2,4-difluorophenyl)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 2.09 (s, 3H), 2.37 (s, 3H), 4.71 (d, J=5.6 Hz, 2H), 6.06 (bs, 1H), 6.47 (bs, 1H), 7.75 (t, J=9.4 Hz, 1H), 7.85 (t, J=10.0 Hz, 1H), 7.17 (t, J=7.3 Hz, 1H), 7.33 (d, J=7.8 Hz, 1H), 7.62 (t, J=7.5 Hz, 1H), 8.12 (bs, 1H), 8.58 (d, J=2.8 Hz, 1H); MS (ESI) m/z 342.6 (M+1)+.

来源

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