تفاعل #91389

ord-ab505874f5de4619825cc64ec6360805

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

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

الإجراء التجريبي

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 {[5-(trifluoromethyl)pyridin-2-yl]methyl}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 light-grey solid. 1H NMR (300 MHz, DMSO-d6) δ ppm 1.04-1.16 (m, 3H), 1.16-1.19 (m, 2H), 1.38 (d, J=10.21 Hz, 2H), 1.55 (s, 3H), 1.86 (s, 3H), 2.26 (bs, 3H) 3.53 (d, J=5.37 Hz, 1H), 4.73 (s, 2H), 7.53 (d, J=7.52 Hz, 2H), 8.15 (d, J=7.79 Hz, 2H), 8.89 (s, 1H), 12.98 (bs, 1H); MS (ESI) m/z 380.0 (M+1)+.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US09447051B2uspto-grants-2016_09