Method for synthesizing 3-amino-4-methacetin by catalytic hydrogenation

Abstract

The invention relates to a method for synthesizing 3-amino-4-methacetin by catalytic hydrogenation, which uses nano-nickle as a catalyst to catalyze 3-nitro-4-methacetin to obtain the 3-amino-4-methacetin through hydrogenation synthesis. The method comprises the following steps: respectively performing ultrasound processing on nickel oxalate and 1 to 50 weight percent of surfactant of the nickel oxalate and dissolving the nickel oxalate and the surfactant thereof into an ethanol solution; then adding the nickel oxalate and the surfactant thereof into a three-neck round-bottomed flask; mixing the nickel oxalate and the surfactant thereof under the stirring of a magnetic stirrer; adjusting the pH value to between 11 and 12; keeping reacting for 1 hour; under the mild stirring, adding a reducing agent of hydrazine hydrate to obtain a nano-nickle catalyst; dissolving the 3-nitro-4-methacetin into the ethanol solution, wherein the consumption of the nano-nickle catalyst is 1 to 20 percent of raw material weight; introducing nitrogen into a reaction kettle to displace air; and introducing the hydrogen into the reaction kettle at a reaction temperature of between 60 and 150 DEG C and at a reaction pressure of between 0.5 and 2.5 Mpa. After the reaction is finished, the conversion rate of the raw material of the 3-nitro-4-methacetin is between 85.5 and 100 percent, and the selectivity of the product of the 3-amino-4-methacetin is between 9.0 and 99.9 percent.

Description

Technical field: [0001] The invention relates to a method for synthesizing 3-amino-4-methoxyacetanilide by catalytic hydrogenation, in particular using nano-nickel as a catalyst to catalyze the hydrogenation of 3-nitro-4-methoxyacetanilide to synthesize 3-amino- 4-Methoxyacetanilide. Background technique [0002] 3-Amino-4-methoxyacetanilide is an important intermediate in the synthesis of azo dyes and drugs, and is a coupling component for the preparation of disperse blue series dyes and disperse dark blue HGL. At present, the production and sales at home and abroad are very large. [0003] Research at home and abroad shows that there are two main ways to prepare 3-amino-4-methoxyacetanilide. One is to use 2,4-dinitrochlorobenzene as raw material, which is prepared by etherification, reduction and acylation. , the etherification product 2,4-diaminoanisole is easily oxidized during this process, and the acylation process is prone to produce 2,4-diacetamidoanisole and 3-ami...

AI Technical Summary

Problems solved by technology

The iron powder reduction method is the most common process. The process is simple and the operation is safe, but it will produce a large amount of iron sludge and waste, which seriously pollutes the environment.

The biggest disadvantage of alkali sulfide reduction is the production of a large amount of industrial wastewater, which has caused great pollution to the environment

Hydrazine hydrate in the hydrazine hydrate reduction method is expensive, highly toxic, low yield and long reaction time

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