تفاعل #91387

ord-6300d0da5fe2457bbd07507ff9dfac54

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-methoxypyridin-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 1.07 (d, J=11.01 Hz, 3H), 1.23 (d, J=11.01 Hz, 2H), 1.47 (d, J=9.94 Hz, 2H), 1.60 (s, 3H), 1.88 (s, 3H), 2.25 (s, 3H), 4.73 (d, J=5.37 Hz, 2H), 7.22-7.29 (m, 2H), 7.59 (d, J=7.79 Hz, 1H), 8.53-8.56 (m, 2H), 12.88 (bs, 1H); MS (ESI) m/z 342.7 (M+1)+.

المصدر

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