Cationic diazo compounds, compositions comprising them, methods for dyeing and kit
A technology of diazo compounds and cations, applied in chemical instruments and methods, azo dyes, onium-based azo dyes, etc., can solve problems such as poor relative tolerance and poor dyeing strength
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Embodiment 1
[0325] Synthesis of the following compounds :
[0326]
[0327] Counter ion: MeSO 4 - / Cl - mixture
[0328] Synthesis reaction process
[0329]
[0330] Counter ion: MeSO 4 - / Cl -
[0331] Compounds 1 and 2 were obtained according to the procedures described in Tetrahedron, 1983, 39(7), 1091-1101 and US 5708151, respectively.
[0332] step
[0333] Compound 2 (15.4 g), compound 1 (16.5 g) and water (150 ml) were poured into a three-necked flask. While stirring, the mixture was heated to 95°C (external temperature).
[0334] After 3.5 hours, the heating was stopped and the mixture was allowed to cool to room temperature.
[0335] The solution was analyzed by chromatography to obtain the expected product.
[0336] After evaporation, a black solid (7.5 g) was obtained.
[0337] NMR and mass spectra were consistent with the structure of the expected product.
[0338] Dyeing example:
[0339] components
quantity
(50 / 50C8 / C10...
Embodiment 2
[0345] Synthesis of compound [8]:
[0346]
[0347] synthetic pathway
[0348] step 1:
[0349]
[0350] Compound [5] is commercially available.
[0351] [4] (5.52 g; 20.67 mmol) was partially dissolved in isopropanol (90 ml) in a three-necked flask equipped with a mechanical stirrer under nitrogen atmosphere, then heated to 60°C. A solution of [5] (7.7 g; 41.34 mmol; 2 eq) dissolved in isopropanol (20 ml) was added by titration. The color of the reaction mixture became very dark red. The reaction mixture was heated at 60 °C overnight and then cooled to room temperature.
[0352] Part of the isopropanol (70ml) was evaporated under vacuum and a precipitate gradually formed.
[0353] The precipitate was filtered, rinsed with isopropanol and dried under vacuum to obtain a green powder [6] (8.15 g; 93%).
[0354] Standard analysis features are consistent with this structure.
[0355] Step 2:
[0356]
[0357] 3-Aminopyridine (0.232 g; 2.46 mmol) was dissol...
Embodiment 3
[0374] Synthesis of compound [10]:
[0375]
[0376] synthetic pathway
[0377] step 1:
[0378]
[0379] 2-Aminoimidazole sulfate is commercially available.
[0380] 2-Aminoimidazole sulfate (0.325 g; 2.46 mmol) was dissolved in 37% hydrochloric acid (0.65 ml), acetic acid (0.65 ml) and water (3.25 ml). The resulting solution was cooled to 0°C and a solution of sodium nitrite (0.170 g; 2.46 mmol) dissolved in water (0.65 ml) was added titration at 0-5°C. The diazotization reaction was ended after 30 minutes.
[0381] Add a small amount of sulfuric acid. The diazonium solution thus obtained was titrated into a solution of [6] (1 g; 2.38 mmol; 0.97 eq.) dissolved in water (20 ml) at 0-5°C. The pH of the solution is 1-2. The cooling bath was removed and the reaction mixture was stirred at room temperature for 2 hours. Its pH was adjusted to 8-9 by titrating 40% aqueous sodium hydroxide solution.
[0382] Precipitate formed, filtered, rinsed with water, diethy...
PUM
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