Monoazo compound as well as product and application thereof
A monoazo compound technology, applied in the field of disperse dyes, can solve the problems of poor dry heat sublimation fastness, poor comprehensive performance, poor compatibility, etc., and achieve good dry heat sublimation fastness, bright color, Good dyebath stability
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Embodiment 1
[0040] Add 15g of ice water and 5.8g of diamine compound represented by formula (II-1) into the reaction flask,
[0041]
[0042] Add 7.1g CNCH dropwise with stirring 2 COOCH 2 CH 3 , Keep the temperature ≤5℃ and react for 4 hours to obtain the compound of formula (Ⅲ-1),
[0043]
[0044] Add 13g of benzoyl chloride dropwise to the reaction flask, adjust the PH=5 with 12g of 30% liquid caustic soda, and control the temperature ≤10℃ to react for 8 hours to obtain the compound of formula (IV-1).
[0045]
[0046] Then, 4g of 30% liquid caustic soda was added dropwise to adjust the system PH≈9.5. Add 7.8g methyl acetoacetate and 6.0g 70% ethylamine aqueous solution, heat to 75℃ and keep the reaction for 12 hours, pour all the reaction liquid into about 200ml cold water, adjust the pH of the system with sulfuric acid <2, naturally cool down, filter, and wash twice with water to obtain 16.2g of the pyridone compound represented by formula (Ⅴ-1),
[0047]
[0048] Add 10.0ml water, 15.2g 30...
Embodiment 2
[0056] Substituting 10.9 g of methanesulfonyl chloride for 13 g of benzoyl chloride in Example 1, 9.4 g of the pyridone compound represented by formula (Ⅴ-2) was prepared.
[0057]
[0058] Substituting the p-nitroaniline represented by the equivalent formula (VI-2) for the o-nitroaniline in Example 1 to obtain the p-nitroaniline diazonium salt,
[0059]
[0060] According to the coupling method in Example 1, the pyridone compound represented by formula (Ⅴ-2) was mixed with an equivalent amount of p-nitroaniline diazonium salt solution to obtain the mono-coupled compound represented by formula (Ⅰ-6) Nitrogen compound 14.1g,
[0061]
[0062] Test data:
[0063] CompoundⅠ-6: Anal.Calcd.for[C 19 H 21 N 5 O 6 S]: C, 51.00; H, 4.73; N, 15.65%. Found: C, 50.91; H, 4.94; N, 15.31%. Main FT-IR absorptions(KBr pellets, cm -1 ): 3420(w), 2224(m), 1687(m), 1640(s), 1591(vs), 1442(s), 1335(m), 837(s).Negative ESI-MS: m / z =447.17,[MH] - .λ max / ε(l·mol -1 ·Cm -1 )=436.5 / 46003 and 310 / 5288.
Embodiment 3
[0065] Substituting 8 g of acetic anhydride for 13 g of benzoyl chloride in Example 1, 11.6 g of the pyridone type heterocyclic compound represented by formula (Ⅴ-3) was prepared.
[0066]
[0067] Substituting 8.4 g of o-nitrop-anisidine represented by formula (VI-1) for the o-nitroaniline in Example 1 to obtain o-nitrop-anisidine diazonium salt,
[0068]
[0069] According to the coupling method in Example 1, the pyridone compound represented by formula (V-3) was mixed with an equivalent amount of o-nitro-p-anisidine diazonium salt solution to obtain the formula (I-8) 19.5g of the monoazo compound shown,
[0070]
[0071] Test data:
[0072] CompoundⅠ-8: Anal.Calcd.for[C 20 H 22 N 6 O 6 ]: C, 54.29; H, 5.01; N, 19.00%. Found: C, 54.06; H, 4.97; N, 18.87%. Main FT-IR absorptions(KBr pellets, cm -1 ): 3450(w), 2225(w), 1683(m), 1620(s), 1504(s), 1465(vs), 1406(m), 1269(m), 1184(m). 1 H NMR(500MHz, CDCl 3 )δ: 15.91(d,1H,NH), 8.07(m,1H,benzene), 7.79(d,1H,benzene), 7.38(m,1H,benzene), 4...
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