Cationic pyridine and pyridazine dyes
A cationic dye technology, applied in the field of cationic pyridine and pyridazine dyes, can solve the problem of reducing the aesthetic value of clothes
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Embodiment 1
[0086] Synthesis of 1,5-dimethyl-2-[(4-dimethylamino)-phenylazo]-pyridine iodide
[0087] (i) Preparation of disperse dye, 5-methyl-2-[(4-dimethylamino)-phenylazo]-pyridine
[0088] 2-Amino-5-picoline (2.16 g) and sodium amide (50 w / w% suspension in toluene, 1.56 g) were added to toluene (60 ml), and the mixture was heated under reflux for 30 minutes. 4-Nitroso-N,N-dimethylaniline (3 g, 0.02 mol) was added in small portions (exothermic reaction) and heating was continued at reflux under argon for 3 hours. After cooling the mixture was evaporated to dryness under reduced pressure to leave a tarry residue which was extracted with hot acetic acid (2 x 100ml). A yield of 2.3 g of reddish-brown insoluble material remained. The acetic acid extract was neutralized by careful addition of sodium hydroxide liquid (40%) to pH 7: this resulted in a color change from purple to brown and the precipitated tarry solid was collected. It was washed several times with water by decantatio...
Embodiment 2
[0093] Synthesis of 1-methyl-2-[(4-dimethylamino)-phenylazo]-quinoline iodide
[0094] (i) Preparation of disperse dye 2-[(4-dimethylamino)-phenylazo]-quinoline
[0095] The scale (0.02 mol) and the method used were similar to those used for the preparation of 5-methyl-2-[(4-dimethylamino)-phenylazo]-pyridine, but with 2-aminoquinoline (2.88 g, 0.02 mol ) instead of 2-aminopyridine. Additionally, a toluene suspension of 2-aminoquinoline and sodium amide was allowed to cool before adding 4-nitroso-N,N-dimethylaniline (3 g, 0.02 mol). After removing the toluene, the residual tar was stirred with dichloromethane and passed through silica gel. The eluate was collected, the solvent was removed and the residue was treated with isopropanol to obtain a brown solid, mp 149-151°C.
[0096] (ii) Preparation of 1-methyl-2-[(4-dimethylamino)-phenylazo]-quinoline iodide
[0097] 2-[(4-Dimethylamino)-phenylazo]-quinoline (1.1 g, 0.004 mol) and iodomethane (11.4 g, 0.08 mol) in ...
Embodiment 3
[0100] UV-Vis spectra were recorded in water buffered to Ph=7 with the dye. Spectra were recorded with an optical density of 1 in a 1 cm cell.
[0101]
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