Compounds for Dyes
A compound and composition technology, applied in the direction of azo dyes, organic dyes, coumarin dyes, etc., to achieve the effect of high thermal stability
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preparation example Construction
[0200] The compound (I) of the present invention can be produced, for example, based on the method described in Dyes and Pigments 2008, 77, 556. Specifically, it can be prepared by subjecting a compound represented by formula (pa1), a compound represented by formula (pa2) and ethyl cyanoacetate to a cyclization reaction in the presence of benzoic acid and a solvent. The reaction temperature is preferably 0°C to 200°C, more preferably 100°C to 150°C. The reaction time is preferably 1 hour to 24 hours, more preferably 8 hours to 18 hours, and still more preferably 8 to 16 hours. Examples of the solvent include methanol, ethanol, 2-propanol, 1-butanol, 1-pentanol, 1-octanol, and N-methylpyrrolidone, among which 1-pentanol is preferred.
[0201]
[0202] [In formula (pa1) and formula (pa2), R 1 ~R 5 , R 7 ~R 9 , A, X and L represent the same meanings as above, respectively. ]
[0203] In the preparation of compound (I), relative to 1 mole of the compound represented by t...
Embodiment
[0436] Next, examples are given to further describe the present invention in detail. Unless otherwise specified, "%" and "part" in an example are mass % and a mass part.
[0437] In the following synthesis examples, the structures of the compounds were confirmed by NMR (JMM-ECA-500; manufactured by JEOL Ltd.) or mass spectrometry (LC; Model 1200, MASS manufactured by Agilent; LC / MSD model manufactured by Agilent).
[0438] The measurement of the weight average molecular weight (Mw) and the number average molecular weight (Mn) of polystyrene conversion of resin was performed on the following conditions by the GPC method.
[0439] Device: HLC-8120GPC (manufactured by Tosoh Co., Ltd.)
[0440] Column; TSK-GELG2000HXL
[0441] Column temperature; 40°C
[0442] Solvent; THF
[0443] Flow rate; 1.0mL / min
[0444] The concentration of solids in the tested liquid; 0.001~0.01% by mass
[0445] Injection volume; 50μL
[0446] Detector; RI
[0447] Calibration standards; TSK poly...
Synthetic example 1
[0452] Mix 10.6 parts of bis(3-amino-4-hydroxyphenyl)sulfone (manufactured by Tokyo Chemical Industry Co., Ltd.), 14.6 parts of 4-(diethylamino) salicylaldehyde (manufactured by Tokyo Chemical Industry Co., Ltd.), benzoic acid (Tokyo Chemical Industry Co., Ltd.) 3.17 parts, 1-pentanol (Tokyo Chemical Industry Co., Ltd.) 183 parts, and ethyl cyanoacetate (Tokyo Chemical Industry Co., Ltd. Hour. 14.6 parts of 4-(diethylamino) salicylaldehyde (manufactured by Tokyo Chemical Industry Co., Ltd.), 3.17 parts of benzoic acid (manufactured by Tokyo Chemical Industry Co., Ltd.) and ethyl cyanoacetate (manufactured by Tokyo Chemical Industry Co., Ltd.) were added to this reaction solution. Co., Ltd.) 8.61 parts, and stirred at 120 degreeC for 12 hours. After cooling the above reaction solution to room temperature, the precipitated crystals were obtained as a residue of suction filtration. After adding 236 parts of acetonitrile and 234 parts of isopropanol to this residue and stirring,...
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