Azabenzotriazol containing ultraviolet absorber and preparation method thereof
A benzotriazole-type, benzotriazole-based technology, applied in the field of nitrogen-containing heterocyclic benzotriazole-type ultraviolet absorbers and their preparation, can solve the problems of weak ultraviolet protection ability and large dosage
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Embodiment 1
[0035] Embodiment 1, a kind of preparation method of nitrogen-containing heterocyclic benzotriazole type ultraviolet absorber, carries out following steps successively:
[0036] 1), the diazotization reaction of p-chloro-o-nitroaniline
[0037] Add 0.1mol of p-chloro-o-nitroaniline to the mixture composed of 0.3mol of concentrated hydrochloric acid and 25ml of water and stir for 0.5~1h, then add 50ml of 2mol / L sodium nitrite aqueous solution dropwise at 0~5℃, and finish adding in 0.5~1h , and keep warm (0-5°C) for 2 hours. After reaching the end of the reaction (that is, after the reaction time is terminated), add a small amount of urea to remove excess nitrous acid; When the test paper does not turn blue rapidly within 3 seconds, it shows that the reaction product does not contain nitrous acid; the resultant is a diazo solution.
[0038] 2), the coupling reaction of p-chloro-o-nitroaniline diazonium salt and N-ethyl-3-cyano-4-methyl-6-hydroxyl-2-pyridone
[0039] After dissol...
Embodiment 2
[0047] Embodiment 2, a kind of preparation method of nitrogen-containing heterocyclic benzotriazole type ultraviolet absorber, carries out following steps successively:
[0048] 1), the diazotization reaction of o-nitroaniline
[0049] Add 0.1mol of o-nitroaniline to the mixture consisting of 0.3mol of concentrated hydrochloric acid and 25ml of water and stir for 0.5~1h, then add 50ml of 2mol / L sodium nitrite aqueous solution dropwise at 0~5°C, finish adding in 0.5~1h, and Keep warm (0-5°C) and react for 3 hours. After reaching the end of the reaction (that is, after the end of the reaction time), add a small amount of urea to remove excess nitrous acid; the end point is detected with starch potassium iodide test paper; when the test paper does not turn blue quickly within 3 seconds, It shows that the reaction product does not contain nitrous acid. The result is diazo solution.
[0050] 2), the coupling reaction of o-nitroaniline diazonium salt and N-ethyl-3-cyano-4-methyl-6...
Embodiment 3
[0057] Embodiment 3, a kind of preparation method of nitrogen-containing heterocyclic benzotriazole type ultraviolet absorber, carries out following steps successively:
[0058] 1), the diazotization reaction of o-nitroaniline
[0059] The diazotization reaction is the same as the step 1) of embodiment 2.
[0060] 2), the coupling reaction of o-nitroaniline diazonium salt and N-butyl-3-cyano-4-methyl-6-hydroxyl-2-pyridone
[0061] Replace the diazo solution obtained in Example 1 with the diazo solution obtained in Example 3 (that is, replace p-chloro-o-nitroaniline diazonium salt with o-nitroaniline diazonium salt), and use N-butyl-3-cyano Base-4-methyl-6-hydroxyl-2-pyridone replaces N-ethyl-3-cyano-4-methyl-6-hydroxyl-2-pyridone, and other coupling reaction conditions are the same as the steps in Example 1 2).
[0062] The product is hydrophobic, directly filtered, washed with water, and dried (80°C) to obtain the coupled product;
[0063] 3), the reduction reaction of th...
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