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G. H. Elgemeie et al.
and neutralized with dilute hydrochloric acid. The precipitated product was
filtered off and recrystallized from absolute ethanol (20 mL).
6a: Yellow, mp 203 8C; yield 90%. nmax/cm21 (KBr), 3271 (NH); 2206 (CN),
1
1735 (CO), 1670 (CO) cm21; H NMR (DMSO) d 1.97 (t, 3H, CH3), 3.74
(s, 2H, CH2), 4.87 (q, 2H,CH2), 7.71–7.96 (m, 5H, C6H5), 9.21 (s, 1H,
NH), and 10.64 (s, 1H, SH). Found: C, 52.35; H, 4.61; N, 8.43%. Calcd. for
C14H14N2O3S2: C, 52.17; H, 4.35; N, 8.70%.
6b: Yellow, mp 220 8C, yield 80%. nmax/cm21 (KBr), 3282 (NH), 2202 (CN),
1
1735 (CO), 1635 (CO) cm21; H NMR (DMSO) d 1.59 (t, 3H, CH3), 2.66
(s, 3H, CH3), 4.37 (s, 2H, CH2), 4.54 (q, 2H,CH2), 7.22–7.62 (m, 4H,
C6H4), 8.12 (s, IH, NH); m/z 336. Found: C, 53.82; H, 4.82; N, 8.51%.
Calcd. for C15H16N2O3S2: C, 53.57; H, 4.76; N, 8.33%.
6c: Yellow, mp 235 8C, yield 85%. nmax/cm21 (KBr), 3275 (NH); 2200 (CN),
1
1700 (CO), 1660 (CO) cm21; H NMR (DMSO) d 1.36 (t, 3H, CH3), 2.82
(s, 3H, OCH3), 3.16 (s, 2H, CH2), 4.33 (q, 2H, CH2), 6.90–7.46 (m, 4H,
C6H4), 7.99 (s, 1H, NH), 12.00 (s, 1H, SH). Found: C, 51.41; H, 4.61; N,
7.63%. Calcd. for C15H16N2O4S2: C, 51.14; H, 4.55; N, 7.95%.
6d: Yellow, mp 233 8C, yield 89%. nmax/cm21 (KBr), 3420 (NH); 2203 (CN),
1
1695 (CO), 1670 (CO) cm21; H NMR (DMSO) d 1.23 (t, 3H, CH3), 3.63
(s, 2H, CH2), 4.17 (q, 2H, CH2), 7.38–7.63 (m, 4H, C6H4), 8.85 (s, 1H,
NH), 10.41 (s, 1H, SH); m/z 358. Found: C, 47.41; H, 3.43; N, 7.58%.
Calcd. for C14H13N2O3S2Cl: C, 47.12; H, 3.65; N, 7.85%.
f[3-(Arylamino)-2-cyano-1-mercapto-3-oxoprop-1-enyl]thiogacetic
Acids 7a–d, General Procedure
a-Chloroacetic acid (0.94 gm, 0.01 mol) was added in portions to a solution
of compounds 3a–d (0.01 mol) in ethanol (20 mL) at room temperature.
The reaction mixture was left for 30 min under stirring, then poured over an
ice–water mixture, and neutralized with dilute hydrochloric acid. The preci-
pitated product was filtered off and recrystallized from ethanol.
7a: Yellow, mp 190 8C, yield 92%. nm.cm21(KBr), 3551, 3417 (OH, NH);
2202 (CN), 1690 (CO), 1675 (CO) cm21. Found: C, 48.63; H, 3.62; N,
9.31% Calcd. for C12H10N2O3S2: C, 48.98; H, 3.40; N, 9.52%.
7b: Yellow, mp 245 8C, yield 84%. nmax/cm21 (KBr), 3460, 3340 (OH, NH);
1
2200 (CN), 1697 (CO), 1670 (CO) cm21; H NMR (DMSO) d 2.29 (s, 3H,
CH3), 4.33 (s, 2H, CH2), 6.20–7.65 (m, 4H, C6H4), 9.50 (s, 1H, NH), 9.90
(s, 1H, SH), 12.31 (s, 1H, OH); m/z 307. Found: C, 50.42; H, 3.72; N,
9.21%. Calcd. for C13H12N2O3S2: C, 50.65; H, 3.90; N, 9.09%.
7c: Yellow, mp 205 8C, yield 81%. nmax/cm21 (KBr), 3400, 3330 (OH, NH);
1
2211 (CN), 1695 (CO), 1655 (CO) cm21; H NMR (DMSO) d 3.97 (s, 3H,