Method for synthesizing 3-amino-4-methoxy acetanilide by binary alloy catalysis

A technology of methoxyacetanilide and binary alloys, which is applied in chemical instruments and methods, preparation of organic compounds, metal/metal oxide/metal hydroxide catalysts, etc., can solve the problem of poor stability and easy agglomeration of nano-metal catalysts , low catalytic activity, etc.

Inactive Publication Date: 2017-01-04
JIANGSU UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, nano-metal catalysts have disadvantages such as poor stability and easy agglomeration.
However, during the activation process of supported nanocatalysts, nanoscale precious metals are easily reduced and easily grow into large-sized metal particles, resulting in low dispersion of active components and low catalytic activity.

Method used

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  • Method for synthesizing 3-amino-4-methoxy acetanilide by binary alloy catalysis
  • Method for synthesizing 3-amino-4-methoxy acetanilide by binary alloy catalysis
  • Method for synthesizing 3-amino-4-methoxy acetanilide by binary alloy catalysis

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Catalyst preparation:

[0029] In the presence of organic modifier CTAB, copper nitrate trihydrate, silver nitrate and hydrazine hydrate were used as raw materials to prepare nano-copper / silver binary alloy catalysts by wet chemical reduction method.

[0030] Dissolve 1.93g of copper nitrate trihydrate and 0.193g of CTAB in 40ml of absolute ethanol, and ultrasonically dissolve them for 30 minutes to form a mixed solution. When the temperature of the mixed solution rises to 60°C, add 1.5mol / L NaOH ethanol solution drop by drop to adjust The pH value of the mixed solution was 8; then dropwise added a dilute ethanol solution of hydrazine hydrate (6ml 85% hydrazine hydrate / 50ml absolute ethanol), and reacted for 2h under magnetic stirring, and cooled the prepared nano-copper to 30 ℃; Weigh 0.27g of silver nitrate and dissolve it in 20ml of absolute ethanol, add the ethanol solution of silver nitrate dropwise to the cooled mixture and react for 1 hour to prepare nano-copper-...

Embodiment 2

[0034] Adopt the same method of embodiment 1 to prepare nano-copper / silver binary alloy catalyst, only change organic modifier to be respectively CA, Tween-80, the process of catalyst catalytic hydrogenation 3-nitro-4-methoxyacetanilide adopts and The same method as in Example 1 can be used to obtain the influence of different modifiers on the catalytic hydrogenation of 3-nitro-4-methoxyacetanilide by preparing nano-copper / silver binary alloy catalysts. The results are shown in Table 1.

[0035] Table 1 Effect of different modifiers on the catalytic hydrogenation of 3-nitro-4-methoxyacetanilide by nano-copper / silver binary alloy catalysts

[0036]

Embodiment 3

[0038] Using the same method as in Example 1 to prepare nano-Cu-Ag catalysts to catalyze the hydrogenation of 3-nitro-4-methoxyacetanilide, only changing the reaction temperature in the kettle to 80°C, 100°C, 140°C and 160°C respectively , the effect of the reaction temperature on the catalytic hydrogenation of 3-nitro-4-methoxyacetanilide can be obtained, and the results are shown in Table 2.

[0039] The influence of table 2 reaction temperature on the catalytic hydrogenation reaction of 3-nitro-4-methoxyacetanilide

[0040]

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Abstract

The invention relates to a method for synthesizing 3-amino-4-methoxy acetanilide by catalytically hydrogenising 3-nitro-4-methoxy acetanilide (NMA) with a nano copper/ silver binary alloy catalyst, and belongs to the field of nano catalysis. The reaction is carried out in a high-pressure reactor, and hydrogen is provided as a hydrogen source under the action of the catalyst. The catalyst has high activity and high selectivity in the reaction process, is unlikely to inactivate, and has good service stability.

Description

technical field [0001] The invention relates to a method for synthesizing 3-amino-4-methoxyacetanilide by catalytic hydrogenation of 3-nitro-4-methoxyacetanilide (NMA) with a nanometer copper / silver binary alloy catalyst, belonging to the field of nanocatalysis . Background technique [0002] 3-Amino-4-methoxyacetanilide is an important intermediate for the synthesis of organic azo-type disperse dyes and some drugs, and can be used to prepare C.I. Disperse Blue 79, C.I. Disperse Blue 301 and Disperse Violet 58. It is the coupling component of dispersing dark blue HGL, and it can also be used in the synthesis of acid dyes, reactive dyes and pigments, and occupies an important position in the industry. my country is the world's largest producer of 3-amino-4-methoxyacetanilide, which has a large demand at home and abroad and has a good market prospect. [0003] The route of traditional industrial production and synthesis of 3-amino-4-methoxyacetanilide starts from chlorobenze...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C231/12C07C233/43B01J23/89
CPCB01J23/8926C07C231/12C07C233/43
Inventor 卢志鹏殷恒波薛武平王爱丽
Owner JIANGSU UNIV
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