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Preparation method for dye intermediate

A dye intermediate and raw material technology, applied in the field of dye intermediate preparation, can solve the problems of reducing the amount of methyl chloroacetate, large proportion of methyl chloroacetate, difficulty in recycling, etc., and achieves improved production efficiency, molar The ratio is small and the effect of omitting the process of reflux and water separation

Inactive Publication Date: 2017-04-19
CHANGSHU CHIKUSHI MACHINERY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The task of the present invention is to provide a kind of preparation method of dyestuff intermediate, and this method can solve the methyl chloroacetate ratio required in the N-alkylation reaction of methyl chloroacetate in the preparation process, the difficulty of recovery and reuse, storage Easy to deteriorate and other problems, and can reduce the use of methyl chloroacetate, thereby significantly reducing production costs and simplifying the production process

Method used

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  • Preparation method for dye intermediate
  • Preparation method for dye intermediate

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Effect test

Embodiment 1

[0014] Add 1mol of m-aminoacetanilide, 3mol of dichloroethane, 1.1mol of methyl chloroacetate and 1.2mol of triethylamine into the reactor, react at 50°C for 7h, then raise the temperature to 70°C, add 10mol of water, stir for 0.5h, After standing still, the water layer was separated, and the solvent was recovered from the organic layer to obtain a dye intermediate with a yield of 93.7% and a purity of 95.9%.

Embodiment 2

[0016] Add 1 mol of 3-(N-methoxyisopropionyl)amino-4-methoxyacetanilide, 5 mol of chlorobenzene, 1.3 mol of methyl chloroacetate and 1.5 mol of triethylamine into the reactor, react at 30°C for 12 hours, Then the temperature was raised to 70°C, 10 mol of water was added, stirred for 0.5 h, the water layer was separated by standing, and the organic layer was recovered from the solvent to obtain a dye intermediate with a yield of 93.5% and a purity of 95.6%.

Embodiment 3

[0018] Add 1mol of 2-amino-4-acetamidoanisole, 10mol of toluene, 1.5mol of methyl chloroacetate and 1.5mol of triethylamine into the reactor, react at 20°C for 18h, then raise the temperature to 70°C, add 10mol of water, Stir for 0.5 h, stand still to separate the water layer, and recover the solvent from the organic layer to obtain a dye intermediate with a yield of 93.8% and a purity of 96.4%.

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Abstract

The invention discloses a preparation method for a dye intermediate and belongs to the technical field of preparation of the dye intermediate. Substituted-aniline shown in the general formula II serves as a raw material, a solvent, methyl chloroacetate and an acid binding agent are added, a reaction is performed for 3-18 h at 20-50 DEG C, then temperature is risen to 70 DEG C, water is added, stirring is performed for 0.5 h, standing is performed so that a water layer can be separated and removed, and after an organic layer recycles the solvent, the dye intermediate as shown by the general formula I can be obtained. The raw material methyl chloroacetate for use is small in mole ratio, the problem that recycled methyl chloroacetate is prone to going bad in the storage process is avoided, the distilling recycling work procedure of the methyl chloroacetate is omitted, the production efficiency is improved, and cost is reduced; and the process is simple, the reaction is mild, the backflow water separation process is omitted, and industrialized production is facilitated.

Description

technical field [0001] The invention belongs to the technical field of preparation of dye intermediates, and in particular relates to a preparation method of dye intermediates. Background technique [0002] Substituted anilines containing -CH2COOCH3 are widely used as a class of important dye intermediates. The commonly used preparation method is to use a large amount of methyl chloroacetate for N-alkylation synthesis in the presence of an acidic agent. Methyl chloroacetate is not only used as a reaction solvent, but also as an alkylating agent and a water-carrying agent. It is used in a large amount, and its molar ratio to the raw material sometimes needs to reach more than 5:1. Methyl chloroacetate is relatively toxic and has a stimulating effect on all tissues of the human body. It is harmful to the body after inhalation, ingestion or absorption through the skin. Simultaneously, the use of a large amount of methyl chloroacetate will inevitably lead to the recovery and re...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C233/43C07C231/12
CPCC07C231/12
Inventor 朱雪忠
Owner CHANGSHU CHIKUSHI MACHINERY