Knoevenagel Condensation of Aldehydes
2109
=
CDCl3) d: 8.23 (1H, s, CH), 7.61 (1H, t, J ¼ 2.01 Hz, aromatic C2-H),
7.46 (1H, td, J ¼ 7.73 Hz and 1.19 Hz, aromatic C6-H), 7.40 (1H, t,
J ¼ 7.87 Hz, aromatic C5-H), 7.10 (1H, qd, J ¼ 7.89 Hz and 1.26 Hz, aro-
matic C4-H), 4.41 (2H, q, J ¼ 7.20 Hz, ꢁOCH2CH3), 1.42 (3H, t,
J ¼ 7.20Hz, ꢁOCH2CH3); 13C NMR (75 MHz, CDCl3) d: 162.47,
156.31, 155.00, 132.66, 130.55, 124.58, 120.95, 116.21, 115.50, 103.02,
62.85, and 14.12. Anal. calcd. for C12H11NO3: C, 66.35; H, 5.10; N,
6.45. Found: C, 66.42; H, 5.05; N, 6.39%.
(E)-Ethyl-2-cyano-2-hexenoate (3q) (entry 17, Table 1): IR (neat):
3436.1, 2964.0, 2232.1, 1734.1, 1626.9, 1270.8, 1073.1, and 758.8 cmꢁ1
=
;
1H NMR (300 MHz, CDCl3) d: 7.67 (1H, t, J ¼ 7.80 Hz, CH), 4.33
(2H, q, J ¼ 7.20Hz, ꢁOCH2CH3), 2.56 (2H, q, J-7.50 Hz, C4-H), 1.62
(2H, sextet, J ¼ 7.50 Hz, C5-H), 1.39 (3H, t, J ¼ 7.20 Hz, ꢁ OCH2CH3),
1.03 (3H, t, J ¼ 7.20 Hz, C6-H); 13C NMR (75 MHz, CDCl3) d: 163.50,
161.30, 113.67, 109.97, 62.38, 33.74, 21.20, 14.06, and 13.66.
2-(2-Chlorophenylmethylene) malononitrile (3t) (entry 20, Table 1): IR
(KBr): 3048.8, 2226.4, 1582.5, 1438.6, 1287.9, 1045.6, 758.1, and
1
617.7 cmꢁ1; H NMR (300 MHz, CDCl3) d: 8.25 (1H, s, CH), 8.16
=
(1H, d, J ¼ 7.76 Hz, aromatic C3-H), 7.56 (2H, d with a small triplet split-
ting at the base, J ¼ 8.16 Hz and 1.30 Hz, aromatic C4-H and aromatic
C6-H), 7.48–7.39 (1H, m, aromatic C5-H); 13C NMR (75 MHz, CDCl3)
d: 155.96, 136.22, 134.95, 130.61, 129.40, 128.96, 127.70, 113.12, 111.82,
and 85.68.
2-(4-N, N-Dimethylaminophenyl methylene) malononitrile (3x) (entry
24, Table 1): IR (KBr): 3435.1, 2924.5, 2203.7, 1613.8, 1522.9, 1358.9,
1183.2, 814.3, and 722.1 cmꢁ1 1H NMR (300 MHz, CDCl3) d: 7.79
;
(2H, d with a small triplet splitting at the base, J ¼ 9.15 Hz and
=
2.88 Hz, aromatic C2-H and aromatic C6-H), 7.42 (1H, s, CH), 6.68
(2H, d with a small triplet splitting at the base, J ¼ 9.22 Hz and
2.82 Hz, aromatic C3-H and aromatic C5-H), 3.13 (6H, s, ꢁNMe2);
13C NMR (75 MHz, CDCl3) d: 157.97, 154.17, 133.71, 119.25, 115.91,
114.84, 111.58, 71.78, and 40.02.
(E)-2-Cyano-3-(3-bromophenyl)2-propenamide (3a0) (entry 27,
Table 1): IR (KBr): 3469.5, 3336.5, 2363.1, 2209.0, 1690.5, 1593.6,
1
1383.4, 1202.2, 781.7, and 673.2 cmꢁ1; H NMR (300 MHz, DMSO-d6)
=
d: 8.13 (1H, s, CH), 8.07 (1H, t, J ¼ 1.64 Hz, aromatic C2-H), 7.89
(1H, brd, J ¼ 7.89 Hz, aromatic C4-H), 7.80 (2H, brs, ꢁCONH2), 7.75
(1H, td, J ¼ 8.06 Hz and 1.01 Hz, aromatic C6-H), 7.49 (1H, t,
J ¼ 8.1 Hz, aromatic C5-H); 13C NMR (75 MHz, DMSO-d6) d: 162.33,
148.97, 134.70, 134.30, 132.26, 131.34, 128.78, 122.27, 116.07, and 108.38.
(2E,4E)-2-Cyano-5-phenyl-2,4-pentadienamide (3b0) (entry 28, Table
1): IR (KBr): 3419.9, 3227.0, 2211.1, 1680.2, 1571.3, 1380.2, 1163.6,
1
982.7 and 752.2 cmꢁ1; H NMR (300 MHz, DMSO-d6) d: 7.95 (1H, d,