Azobenzol dye compound and preparation thereof
A dye compound and azobenzene technology, applied in the field of azobenzene dye compounds and their preparation, can solve the problem that the photochromic process of the azo chromophore is not easy to control, and achieves improved stability, controllability and broad application. Foreground effect
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Embodiment 1
[0030] Example 1: Preparation of 2-methyl-2'-hydroxyl-3'-tert-butyl-5'-methylazobenzene
[0031] 1. Preparation of diazonium salt
[0032] In a 250mL three-necked bottle equipped with a stirrer and a thermometer, add 10.6g of o-methylaniline, 25mL of 36% hydrochloric acid, 15mL of 36% acetic acid and 75mL of water, place the three-necked bottle in an ice-salt bath, and add 25mL of 30% Keep the reaction temperature below 5°C, react for 1.5 hours, remove excess sodium nitrite with urea, and obtain a purple-red diazonium salt solution.
[0033] 2. Coupling reaction
[0034] Add 1.69g of o-tert-butyl-p-cresol and 25mL of water into a 500mL three-necked flask, and simultaneously add diazonium salt solution and 1mol / L Na 2 CO 3 Aqueous solution 150mL, control pH ≈ 7.5, react for 5h, then raise the temperature to 70°C, react for 2h, acidify with dilute hydrochloric acid to pH = 2, wash with water, filter, and vacuum dry at 80°C to obtain a crude product. Recrystallization with a ...
Embodiment 2
[0043] Example 2: Preparation of 2-nonyl-2'-hydroxyl-3'-tert-butyl-5'-methylazobenzene
[0044] 1. Preparation of diazonium salt
[0045]In a 250mL three-necked flask equipped with a stirrer and a thermometer, add 21.9g of 2-nonylaniline, 15mL of 36% sulfuric acid, 15mL of 36% acetic acid and 75mL of water, place the three-necked flask in an ice-salt bath, and add 28mL of 30 % sodium nitrite aqueous solution, keep the reaction temperature not exceeding 5°C, react for 1.5h, and remove the excess sodium nitrite with urea to obtain a purple-red diazonium salt solution.
[0046] 2. Coupling reaction
[0047] Add 1.94g of o-tert-butyl-p-cresol and 25mL of water into a 500mL three-necked flask, and simultaneously add diazonium salt solution and 2mol / L Na 2 CO 3 Aqueous solution 150mL, control pH ≈ 7.5, react for 5h, then raise the temperature to 70°C, react for 2h, acidify with dilute hydrochloric acid to pH = 2, wash with water, filter, and vacuum dry at 80°C to obtain a crude p...
Embodiment 3
[0050] Example 3: Preparation of 2-methyl-2'-hydroxyl-3'-methyl-5'-methylazobenzene
[0051] 1. Preparation of diazonium salt
[0052] In a 250mL three-necked bottle equipped with a stirrer and a thermometer, add 10.6g of o-methylaniline, 30mL of 36% hydrochloric acid, 15mL of 36% acetic acid and 75mL of water, place the three-necked bottle in an ice-salt bath, and add 23mL of 30% Keep the reaction temperature below 5°C, react for 1.5 hours, remove excess sodium nitrite with urea, and obtain a purple-red diazonium salt solution.
[0053] 2. Coupling reaction
[0054] Add 1.28g of o-methyl-p-cresol and 25mL of water into a 500mL three-necked flask, and simultaneously add diazonium salt solution and 2mol / L Na 2 CO 3 Aqueous solution 150mL, control pH ≈ 7.5, react for 7 hours, acidify with dilute hydrochloric acid to pH = 2, wash with water, filter, and vacuum dry at 80°C to obtain a crude product. Recrystallization with a mixed solvent of ethanol and water at a volume ratio ...
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