تفاعل #91386

ord-644c41c40e514b22aed100b4c55e06b8

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 (4-methylpyridin-2-yl)methanamine 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 0.92-1.67 (m, 10H), 1.88 (s, 3H), 2.28 (s, 3H), 2.53 (s, 3H), 3.63 (bs, 1H), 4.92 (d, J=4.30 Hz, 2H), 7.60-7.80 (m, 3H), 8.19 (bs, 1H), 8.66 (d, J=5.64 Hz, 1H), 13.34 (s, 1H); MS (ESI) m/z 326.0 (M+1)+.

المصدر

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