Med Chem Res
2-(4-Nitrophenyl) isoindoline-1,3-dione (3)
N-(4-(1,3-Dioxoisoindolin-2-yl) phenyl) acetamide (7)
Preparation of this compound has been reported already
(Vamecq et al., 2000). By means of the general procedure,
3-nitroaniline provided the title compound after 10 h of
reflux: yellow crystals, yield 81.5 %; mp 262–264 °C
(ethanol). IR (KBr): m cm-1, 3119 (CH-aromatic), 1780,
1731 (CO), 1521, 1347 (NO2); 1H NMR (CDCl3): d 8.35(d,
J = 9.18 Hz, 2H, H3,5-phenyl), 7.71–7.94(m, 6H, aro-
matic); Mass m/z (rel.int): 268 (M?, 43), 237 (21), 165
(14), 103 (36), 74 (100), Anal. Calcd. for C14H8N2O4: C,
62.69; H, 3.01; N, 10.44. Found: C, 62.57; H, 3.00; N,
10.42.
By means of the general procedure, N-(4-aminophenyl)
acetamide provided the title compound after 20 h of reflux:
violet crystals, yield 85 %; mp 228–231 °C (methanol). IR
(KBr): m cm-1, 3318 (NH), 3020 (CH-aromatic), 2919 (CH-
aliphatic), 1787, 1710, 1675 (CO); 1HNMR (DMSO-d6): d
9.87(br, 1H, NH), 7.79–7.89(m, 4H, aromatic), 7.70(d,
J = 8.78 Hz, 2H, H3,5-phenyl), 7.28 (d, J = 8.9 Hz, 2H,
H
2,6-phenyl), 2.12 ppm (s, 3H, CH3); Mass m/z (rel.int): 280
(M?, 22), 238 (29), 236 (43), 177 (14), 130 (6), 103 (50), 75
(100); Anal. Calcd. for C16H12N2O3: C, 68.56; H, 4.32; N,
9.99. Found: C, 68.49; H, 4.33; N, 9.97.
2-(1, 3-Dioxoisoindolin-2-yl) benzoic acid (4)
4-(1,3-Dioxoisoindolin-2-yl) benzene sulfonamide (8)
By means of the general procedure, 2-aminobenzoic acid
provided the title compound after 8 h of reflux: White
crystals, yield 61 %; mp 217–221 °C (chloroform). IR
(KBr): m cm-1, 3200 (OH), 3083 (CH-aromatic), 1721,
By means of the general procedure, 4-aminobenzenesulf-
onamide provided the title compound after 55 h of reflux:
yellow crystals, yield 89 %; mp 185–187 °C (methanol).
IR (KBr): m cm-1, 3365, 3257 (NH2), 1721, 1680 (CO),
1
1698 (CO); H NMR (DMSO-d6): d 8.16 (dd, J = 6.60,
1
1301, 1157(SO2); H NMR (DMSO-d6): d 7.96–8.09 (m,
2.30 Hz, 1H, H3-phenyl)), 7.41–7.95 ppm (m, 7H, aro-
matic); Mass m/z (rel.int): 268 (M? ?1, 18), 266(M?- 1,
100), 221 (100), 195 (50), 177 (100), 102 (48), 139 (28),
104 (100), 74 (100), 49 (100); Anal. Calcd. for C15H9NO4:
C, 67.42; H, 3.39; N, 5.24. Found: C, 67.51; H, 3.40; N,
5.23.
6H, aromatic), 7.68 (d, J = 8.27 Hz, 2H, H2,6-phenyl),
7.28 ppm (s, 2H, NH2); Mass m/z (rel.int): 302(M?, 29),
301 (M?-1, 36), 237 (14), 222 (78), 166 (21), 103 (50), 75
(100); Anal. Calcd. for C14H10N2O4S: C, 55.62; H, 3.33; N,
9.27. Found: C, 55.72; H, 3.34; N, 9.25.
5-(1,3-Dioxoisoindolin-2-yl)-1,3,4-thiadiazole-2-
sulfonamide (9)
4-(1,3-Dioxoisoindolin-2-yl) benzoic acid (5)
By means of the general procedure, 4-aminobenzoic acid
provided the title compound after 17 h of reflux: White
crystals, yield 80 %; mp 282–289.5 °C (ethanol). IR
(KBr): m cm-1, 3225–3310 (OH), 3067 (CH-aromatic),
By means of the general procedure, 5-amino-1,3,4-thia-
diazole-2-sulfonamide provided the title compound after
5 h of reflux: White crystals, yield 47 %; mp 264–274 °C
(ethanol). IR (KBr): m cm-1, 3329, 3180 (NH2), 3078 (CH-
aromatic), 1792, 1736 (CO); 1H NMR (DMSO-d6): d
7.90–8.02(m, 4H, aromatic); Mass m/z (rel.int): 310 (M?,
14), 308 (30), 244 (25), 188 (9), 170 (33), 156 (10), 102
(58), 74 (100); Anal. Calcd. for C10H6N4O4S2: C, 38.71; H,
1.95; N, 18.06. Found: C, 38.82; H, 1.94; N, 18.04.
1
1726, 1695 (CO); H NMR (DMSO-d6): d 8.42–9.51 (brs,
1H, COOH), 8.17 (d, J = 8.58 Hz, 2H, H3,5-phenyl),
7.75–8.03 (m, 4H, aromatic), 7.56 ppm (d, J = 8.58 Hz,
2H, H2,6-phenyl);. Anal. Calcd. for C15H9NO4: C, 67.42;
H, 3.39; N, 5.24. Found: C, 67.55; H, 3.40; N, 5.25.
2-Hydroxy-4-(1,3-dioxoisoindolin-2-yl) benzoic acid (6)
2-(4-Methoxy-2-nitrophenyl) isoindoline-1,3-dione (10)
By means of the general procedure, 4-amino-2-hydroxy-
benzoic acid provided the title compound after 2 h of reflux:
White crystals, yield 40 %; mp 293–295 °C (methanol–
chloroform). IR (KBr): m cm-1 2750–3700 (OH), 1716,
By means of the general procedure, 4-methoxy-2-nitroan-
iline provided the title compound after 7 h of reflux: yellow
crystals, yield 62.5 %; mp 148–153 °C (ethanol). IR
(KBr): m cm-1, 3080 (CH-aromatic), 2938 (CH-aliphatic),
1
1676 (CO); HNMR (DMSO-d6): d 11.25–1155 (brs, 1H,
1
1781, 1723 (CO), 1540, 1387(NO2); H NMR (CDCl3): d
COOH), 7.75–8.12 (m, 5H, aromatic), 7.06–7.39 ppm (m,
2H, H2,6-phenyl); Mass m/z (rel.int): 283 (M?, 25), 265
(60), 237 (19), 192(10), 132 (31), 103 (65), 76 (72), 75
(100).; Anal. Calcd. for C15H9NO5: C, 63.61; H, 3.20; N,
4.95. Found: C, 63.70; H, 3.21; N, 4.96.
7.69–7.93 (m, 4H, aromatic), 7.60 (d, J = 2.56 Hz, 1H,
H3-phenyl), 7.24(d, J = 8.5 Hz, 1H, H6-phenyl), 7.16 (dd,
J = 8.70, 2.6 Hz, 1H, H5-phenyl), 3.83 ppm (s, 3H,
OCH3); Mass m/z (rel.int): 298 (M?, 38), 252 (100), 209
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