Heterocyclic-ring disperse azo dye and preparation method thereof
A technology of disperse dyes and heterocyclic azo, applied in the direction of azo dyes, monoazo dyes, dyeing methods, etc., can solve problems such as difficulty in obtaining dyes
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[0138] On the other hand, the present invention also provides the preparation method of above-mentioned compound, and this preparation method is to carry out diazotization to diazonium component in organic solvent in the presence of concentrated sulfuric acid, precipitates stable diazonium salt solid, After the solid is obtained by filtration, the coupling reaction with the coupling component is carried out under alkaline conditions to obtain the target dye. Specifically include the following steps:
[0139] (1) Add the diazo component, concentrated sulfuric acid, organic solvent and stabilizer described in the present invention into the reaction vessel A, after cooling down to 0-10°C, add the diazotization reagent in batches, react for 0.1-10h, and filter Obtain the diazonium salt solid of diazo component;
[0140] (2) Add the coupling component and water according to claim 1 into the reaction vessel B, adjust the pH value to 8-12 with 10% sodium hydroxide, dissolve the coup...
Embodiment 1
[0151] The preparation of embodiment 1 compound 1#
[0152] (1) Add 1.5g of 5-aminobenzimidazolone, 1g of concentrated sulfuric acid, 80ml of ethylene glycol diethyl ether, and 5g of 1,5-naphthalene disulfonic acid into a three-necked flask, cool down to 5°C in an ice-water bath, and add 3g of nitrous acid dropwise tert-butyl ester, the dropping time is 0.5h, and react for 2 hours after the dropping is completed; the diazonium salt solid is obtained after filtration; (2) 1.34g 3-methyl-1-phenyl-5 pyrazolone, 100ml water Add it into the reactor, adjust the pH value to 10 with 10% sodium hydroxide solution, cool to 5 ° C, add the 5-aminobenzimidazolone diazonium salt obtained in step (1) under stirring, and control the pH value with 10% sodium carbonate solution The pH value is 9, the addition is completed within half an hour, and the reaction is carried out at 5°C for 2 hours; the reaction is completed, filtered, washed with ice water until the filtrate is neutral, and dried to...
Embodiment 2
[0155] The preparation of embodiment 2 compound 2#
[0156] (1) Add 1.83g of 2,4-dinitroaniline, 2g of concentrated sulfuric acid, 40ml of ethylene glycol dimethyl ether, and 4g of 1,5-naphthalene disulfonic acid into a three-necked flask, cool down to 3°C in an ice-water bath, and drop 3g Nitrosyl sulfuric acid, the dropping time is 0.5h, and react for 2 hours after the dropping is completed; after filtration, the diazonium salt solid is obtained; (2) Add 0.81g of 3-methyl-5-pyrazolone and 80ml of water into the reactor , adjust the pH value to 11 with 10% sodium hydroxide solution, cool to 4 ° C, add the 2,4-dinitroaniline diazonium salt obtained in step (1) under stirring, and use 10% sodium carbonate solution to control the pH value at 9. Complete the addition within half an hour, and react at 5°C for 2 hours; after the reaction is completed, filter, wash with ice water until the filtrate is neutral, and obtain a heterocyclic azo disperse dye (compound 2#) after drying, wi...
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