Chemical synthesis method of phthalimide structure containing coupling components and disperse dyes
A technology of phthalimide and coupling components, which is applied in the field of chemical synthesis of disperse dyes, and can solve problems such as the preparation method of unpublished phthalimide structure coupling components, etc.
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Embodiment 1
[0058] Add 10.9g of N-methylaniline (purity 98%, 0.1mol), acrylic acid 7.3g (purity 98%, 0.1mol), toluene 180g, p-toluenesulfonic acid 0.5g into a three-necked flask, and heat to 70°C React for 9 hours, cool down, add 18.3g of N-2-hydroxyethylphthalimide (98% purity, 0.1mol), 0.2g of 98% concentrated sulfuric acid, add 180g of toluene, and heat to 100°C Reacted for 18 hours, lowered the temperature, and distilled off the solvent toluene under reduced pressure to obtain 34.7 g of a coupling component with a structure as shown in (I-1), with a purity of 89.4% and a yield of 88.3% (as N-methyl aniline meter).
[0059] Add 9.5g of concentrated sulfuric acid (purity 98%, 0.095mol) to a three-necked flask, cool it down to 0°C with an ice bath, stir, and slowly add 6.5g of sodium nitrite (purity 98.5%, 0.093mol) to keep the temperature at 0°C and stir for 1 hour, slowly add diazo component 2-cyano-4-nitroaniline 14.8g (purity 98%, 0.089mol), continue to stir for 5 hours, then slowly...
Embodiment 2
[0063] Add 18.0g of 3-acetamido-N-ethylaniline (purity 99%, 0.1mol), acrylic acid 9.2g (purity 98%, 0.125mol) into a three-necked flask, no solvent is added, and the catalyst is 0.28g of methanesulfonic acid , heated to 120°C and reacted for 3 hours, cooled down, added solvent xylene 400g, added N-2-hydroxyethylphthalimide 23.8g (purity 98%, 0.13mol), 98% concentrated sulfuric acid 0.3g, reacted under reflux for 5 hours, lowered the temperature, and distilled off the solvent toluene under reduced pressure to obtain 43.4g of a coupling component with the structure shown in (I-2), with a purity of 85.6% and a yield of 87.7% according to high performance liquid chromatography (as 3-acetamido-N-ethylaniline).
[0064] All the other operations are the same as in Example 1, and 55.3 g (dried) of a phthalimide structure-containing disperse dye filter cake having a structure as shown in (IX-2) is obtained, and the HPLC analysis purity is 92.1%, and the yield 95.3% (calculated as diaz...
Embodiment 3
[0068] Add 14.5g of 2-chloro-N-methylaniline (purity 98%, 0.1mol), 4-chlorobutyric acid 18.8g (purity 98%, 0.15mol), solvent DMF 665g, and catalyst sodium hydroxide in a three-necked flask 1.66g, heated to 150°C and reacted for 6 hours, lowered the temperature, added solvent DMF 365g, and the rest of the operation was the same as in Example 1 to obtain 39.7g of the coupling component shown in (I-3), and the purity was analyzed by high performance liquid chromatography It was 90.3%, and the yield was 89.2% (based on 2-chloro-N-methylaniline).
[0069] All the other operations are the same as in Example 1. After the diazo coupling reaction, 53.8 g of disperse dye filter cakes containing phthalimide structure (dried) with a structure as shown in (IX-3) are obtained, and analyzed by high performance liquid chromatography. The purity is 90.6%, and the yield is 94.8% (based on diazo components).
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