116
D. S. REKUNGE ET AL.
General procedure for the synthesis of 2-Amino-4,6-(disubstituted)nicotinonitriles
(5a-x)
A mixture of substituted aldehyde (2 mmol), substituted acetophenone (2 mmol), malo-
nonitrile (2 mmol), ammonium acetate (2.4 mmol), and activated Fuller’s earth (20 wt.
%) was heated at 90 ꢀC in an oil bath. The reaction was monitored by thin-layer chro-
matography. After completion of the reaction, the reaction mass was treated with hot
ethanol (5 mL) dissolving the organic product and leaving the Fuller’s earth insoluble.
The Fuller’s earth was removed by hot filtration. The filtrate was evaporated to get the
product. The product was purified by recrystallization from ethanol.
2-Amino-4-(2-nitrophenyl)-6-phenylnicotinonitrile (5k)
1H NMR (400 MHz, DMSO-d6) d 8.23 (d, J ¼ 8.2 Hz, 1H), 8.12 – 8.02 (m, 2H), 7.94 –
7.85 (m, 1H), 7.79 (dd, J ¼ 17.7, 9.6 Hz, 1H), 7.64 (d, J ¼ 7.6 Hz, 1H), 7.45 (d, J ¼
3.1 Hz, 3H), 7.24 (s, 1H), 7.10 (s, 2H). HRMS calculated for C18H12N4O2: 316.09602;
found: (MHþ) 317.10234 m/z.
2-Amino-6-(3-bromophenyl)-4-phenylnicotinonitrile (5q)
1H NMR (400 MHz, DMSO-d6) d 8.33 (s, 1H), 8.11 (d, J ¼ 8.0 Hz, 1H), 7.65 (m, 3H),
7.52 (d, J ¼ 6.8 Hz, 3H), 7.41 (t, J ¼ 7.6 Hz, 1H), 7.32 (s, 1H), 7.04 (s, 2H). HRMS calcu-
lated for C18H12BrN3: 349.02145; found: (MHþ) 350.02764 m/z.
2-Amino-6-(3-bromophenyl)-4-(4-methoxyphenyl)nicotinonitrile (5v)
1H NMR (400 MHz, DMSO-d6) d 8.32 (m, 1H), 8.10 (s, 1H), 7.65-7.63 (m, 2H), 7.43-
7.41 (m, 1H), 7.08-6.98 (m, 4H), 3.81 (s, 3H). HRMS calculated for C19H14BrN3O:
379.03202; found: (MHþ) 382.03616 m/z.
2-Amino-6-(3-bromophenyl)-4-(p-tolyl)nicotinonitrile (5w)
1H NMR (400 MHz, DMSO-d6) d 8.35 (s, 1H), 8.13 (d, J ¼ 7.8 Hz, 1H), 7.67 (d,
J ¼ 7.9 Hz, 1H), 7.59 (d, J ¼ 7.9 Hz, 2H), 7.45 (t, J ¼ 7.9 Hz, 1H), 7.36 (d, J ¼ 7.9 Hz, 2H),
7.32 (s, 1H), 7.06 (s, 2H), 2.40 (s, 3H). HRMS calculated for C19H14BrN3: 363.03710;
found: (MHþ) 364.04324 m/z.
2-Amino-4,6-bis(3-bromophenyl)nicotinonitrile (5x)
1H NMR (400 MHz, DMSO-d6) d 8.34 (s, 1H), 8.13 (d, J ¼ 8.8 Hz, 1H), 7.86 (s, 1H),
7.71 (d, J ¼ 8.0 Hz, 1H), 7.65 (t, J ¼ 7.2 Hz, 2H), 7.50-7.42 (m, 2H), 7.35 (s, 1H), 7.09 (s,
2H). HRMS calculated for C18H11Br2N3: 426.93196; found: (MHþ) 429.3570 m/z.
Acknowledgment
The authors are grateful to the University Grant Commission, New Delhi, for their finan-
cial support.