Synthesizing method of dye intermediate with N-acetic ester group structure

Abstract

The invention discloses a synthesizing method of a dye intermediate with an N-acetic ester group structure. The synthesizing method comprises the steps of conducting reflux reaction on substituted aniline, chloroacetic ester and an acid-binding agent for 0.5-2.0 hours at the temperature of 80-110 DEG C, adding a catalyst and zinc powder, and further conducting water separation reflux reaction for1.0-3.0 hours at the temperature of 105-130 DEG C to obtain the dye intermediate. The dye intermediate can be directly applied to dye synthesis. The synthesizing method has the advantages that the catalytic reaction speed is high, the product purity (HPLC) reaches 99% or above, and the yield reaches 98% or above. The synthesizing method is particularly suitable for synthesizing the dye intermediate containing the N,N-diacetic ester group with the purity higher than 99%.

Description

technical field [0001] The invention relates to a synthesis method of a dye intermediate, in particular to a synthesis method of a dye intermediate with an N-acetate group structure, and belongs to the technical field of dyes. Background technique [0002] Aromatic amines substituted with N-ester groups are an important class of disperse dye intermediates, and there are mainly three synthetic methods. The first method is that the amino group of the aromatic amine is hydroxyethylated with ethylene oxide, and then esterified with acetic acid or acetic anhydride. For example, the coupling component of disperse blue 79 was synthesized from 2-methoxy-5-acetamidoaniline. The second method is that the amino group of the aromatic amine is obtained by addition of an alkylating agent containing a propionate group. For example, the addition reaction of 2-methoxy-5-acetamidoaniline and methyl acrylate, the addition reaction of aniline and methyl acrylate. The third method is that the...

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Problems solved by technology

For example, Chinese patent (CN106565528A) discloses that benzene-based solvents are used as water-carrying agents, organic amines are used as acid-binding agents, and aromatic amines and methyl chloroacetate are subjected to N-alkylation reactions. This method has a low reaction temperature and a long time, and is applicable to Synthesize dye intermediates with a monoacetate structure, the resulting dye intermediates containing methyl monoacetate have a purity of 96%, but for dye intermediates with a diacetate structure, as well as ethyl acetate, acetic acid The dye intermediate of propyl ester group has no embodiment report

Chinese patent (CN 102633666A) is aimed at the current containing methyl acetate group (-CH 2 COOCH 3 ) of the substituted aniline dye intermediates in the synthesis process requires a large proportion of methyl chloroacetate, difficulty in recycling, and easy deterioration in storage. N-alkylation reaction with methyl chloroacetate at reflux temperature to synthesize dye intermediate with diacetate structure

However, the reaction time of these techniques is longer, generally about 8 hours, and the resulting dye intermediate purity containing diacetate group is about 96% (HPLC), and there is no synthetic dye intermediate containing ethyl acetate group The example report

There is no literature report that can obtain more than 99% high-purity N,N-diacetate-based dye intermediates

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