Quinaldine based semisquaraines and squaraine dyes, process for preparation thereof and use thereof
A technology of squarylium and quinaldine, applied in the field of quinaldine-based semisquarine and squarylium dyes, their preparation and application, capable of solving problems such as the difficulty of destroying deep tumors
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Embodiment 1
[0063] General procedure for preparing the compound represented by Formula 1. The corresponding mixture of quinalidine salt (1mmol), square acid (1mmol) and quinoline (0.5mL) in a mixture of n-butanol and benzene (6-9mL each, 1:1) in azeotropic distillation with water Reflux for 24-36h under conditions. The solvent was distilled off under reduced pressure to obtain a residue, which was chromatographed on silica gel. The column was eluted with a mixture of methanol and chloroform (1:19) to obtain the hemisquaraine of general formula 1.
[0064] General formula 1 (where X=OH, Y=H and Z=H, R 2 =CH 3 , 90-95%) of the physical and chemical properties of the compound: mp 150-152℃, IR(KBr)v max 3412, 3042, 2963, 1761, 1606cm -1 . 1 H-NMR(CDCl 3 +DMSO-d 6 , 1:4) δ 10.06 (1H, OH), 9.29 (1H, d, J = 11.4 Hz), 7.89 (1H, d, J = 9.3 Hz), 7.73 (1H, d, J = 9.4 Hz), 7.34 (1H, d, J = 9.3 Hz), 7.17 (1H, s), 6.14 (1H, s), 4.64 (2H, t, J = 6.5 Hz), 4.11 (3H, s), 1.78 (2H, m) , 1.45 (2H, m), 0.93 (3H, ...
Embodiment 2
[0069] General procedure for preparing the compound represented by Formula 2. The mixture of the corresponding quinalidine salt (1mmol), squaric acid (0.5mmol) and quinoline (0.5mL) was azeotropically distilled with water in a mixture of n-butanol and benzene (6-9mL each, 1:1) Reflux for 24-36h under the same conditions. The solvent was distilled off under reduced pressure to obtain a residue, which was chromatographed on silica gel. The column was eluted with a mixture of methanol and chloroform (1:9) to obtain the corresponding squaraine dye of general formula 2.
[0070] General formula 2 (where X=Br, Y=H, R 2 =CH 3 , 90-95%) of the physical and chemical properties of the compound: mp 336-338℃, IR(KBr)v max 3056, 1613, 1580cm -1 . 1 H-NMR(DMSO-d 6 )δ 9.31 (1H, d, J=9.5 Hz), 9.28 (1H, d, J=9.3 Hz), 7.3-8.4 (8H, m, aromatic), 5.86 (1H, s, ethylene), 5.78 (1H, s, ethylene), 3.85 (3H, s); 3.78 (3H, s); FAB-MS: m / z=550.246 (C 26 H 18 Br 2 N 2 O 2 The calculated value is 550.248).
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Embodiment 3
[0077] General procedure for preparing the compound represented by Formula 3. Mix the corresponding hemisquaraine (1mmol) and iodine or bromine substituted quinalidine salt (1mmol) and quinoline (0.5mL) in a mixture of n-butanol and benzene (6-9mL each, 1:1) Reflux for 18-24h under conditions of azeotropic distillation with water. The solvent was distilled off under reduced pressure to obtain a residue, which was chromatographed on silica gel. The column was eluted with a mixture of methanol and chloroform (1:9) to obtain the corresponding squaraine dye.
[0078] General formula 3 (where X=OH, Q=I, Y=H, Z=H, R 2 =CH 3 , 90%) of the physical and chemical properties of the compound: 325℃, IR(KBr)v max 3442, 3046, 1729, 1621, 1579, 1560cm -1 . 1 H-NMR(DMSO-d 6 )δ 10.2 (1H, OH), 9.29 (1H, d, J = 9.2 Hz), 9.01 (1H, d, J = 9.5 Hz), 7.86-7.01 (8H, m), 5.77 (1H, s, ethylene ), 5.44 (1H, s, ethylene), 3.9 (3H, s), 3.5 (3H, s); FAB-MS: m / z=534.040 (C 26 H 19 IN 2 O 3 The calculated value is...
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