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...

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