Method for preparing 3-amino-4-methoxyacetanilide by taking Raney nickel as catalyst

A technology of methoxyacetanilide and Raney nickel, which is applied in the direction of Raney catalysts, chemical instruments and methods, and the preparation of organic compounds, can solve environmental pollution and other problems, and achieve a green reaction process, high catalyst activity, Effect of high feedstock conversion and product selectivity

Inactive Publication Date: 2010-11-10
JIANGSU UNIV
View PDF2 Cites 15 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Most of the industrialized preparation of 3-amino-4-methoxyacetanilide in my cou

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Method for preparing 3-amino-4-methoxyacetanilide by taking Raney nickel as catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Add the Ni-Al alloy with a mass ratio of 1:1 to 150mL of 20wt.% sodium hydroxide solution at 50°C within 5min, heat to 80°C after the addition, and keep it at 80°C for 90min, the whole process maintains Stirring state. After the reaction, cool down, filter, wash the filter cake with ethanol three times and then wash with distilled water until pH = 7, and finally store the prepared Raney nickel in absolute ethanol for future use. Weigh 1.0 g of the Raney nickel catalyst prepared above, 10 g of 3-nitro-4-methoxyacetanilide, that is, the mass ratio of the catalyst to the raw material is 1:10, add them to a 1000 mL reactor, add 200 mL of methanol, and start Stir. Nitrogen was introduced for 10 minutes to fully replace the oxygen in the reactor, and hydrogen was added to make the pressure 0.8MPa. Then, gradually raise the temperature to 80°C and react for 2h. After the reaction, the reactor was cooled to about 30°C, and samples were taken for liquid chromatography detecti...

Embodiment 2

[0019] Add the Ni-Al alloy with a mass ratio of 1:2 to 150mL of 20wt.% sodium hydroxide solution at 50°C within 20min, heat it to 80°C after the addition, and keep it at 80°C for 120min, the whole process maintains Stirring state. After the reaction, cool down, filter, wash the filter cake with ethanol three times and then wash with distilled water until pH = 7, and finally store the prepared Raney nickel in absolute ethanol for future use. Weigh 1.0 g of the Raney nickel catalyst prepared above, 10 g of 3-nitro-4-methoxyacetanilide, that is, the mass ratio of the catalyst to the raw material is 1:10, add them to a 1000 mL reactor, add 200 mL of methanol, and start Stir. Nitrogen was introduced for 10 minutes to fully replace the oxygen in the reactor, and hydrogen was added to make the pressure 2.0 MPa. Then, gradually raise the temperature to 100°C and react for 2h. After the reaction, the reactor was cooled to about 30°C, and samples were taken for liquid chromatography ...

Embodiment 3

[0021] Add the Ni-Al alloy with a mass ratio of 1:4 to 150mL of 20wt.% sodium hydroxide solution at 50°C within 5min, heat to 80°C after the addition, and keep it at 80°C for 100min, the whole process maintains Stirring state. After the reaction, cool down, filter, wash the filter cake with ethanol three times and then wash with distilled water until pH = 7, and finally store the prepared Raney nickel in absolute ethanol for future use. Weigh 1.0 g of the Raney nickel catalyst prepared above, 10 g of 3-nitro-4-methoxyacetanilide, that is, the mass ratio of the catalyst to the raw material is 1:10, add them to a 1000 mL reactor, add 200 mL of methanol, and start Stir. Nitrogen was introduced for 10 minutes to fully replace the oxygen in the reactor, and hydrogen was added to make the pressure 1.5 MPa. Then, gradually raise the temperature to 110°C, and react for 2h. After the reaction, the reactor was cooled to about 30°C, and samples were taken for liquid chromatography det...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

No PUM Login to view more

Abstract

The invention discloses a method for preparing 3-amino-4-methoxyacetanilide by catalytic hydrogenation of Raney nickel. In the method, Raney nickel is used as a catalyst for efficiently catalyzing 3-nitro-4-methoxyacetanilide to be reduced into the 3-amino-4-methoxyacetanilide. At the reaction temperature of between 80 and 110 DEG C, under the reaction pressure of 0.8 to 2 MPa and in the reaction time of 2 to 6 h, the 3-amino-4-methoxyacetanilide is prepared from the 3-nitro-4-methoxyacetanilide by liquid phase intermittent catalytic hydrogenation; and the material conversion rate is 85.1 to 100 percent, and the selectivity of the product 3-amino-4-methoxyacetanilide is 99.0 to 99.6 percent. The method has the advantages of clean process, low cost, high purity of the prepared product, safe and environment-friendly process and easy industrialized production.

Description

technical field [0001] The invention relates to a method for preparing 3-amino-4-methoxyacetanilide using Raney nickel as a catalyst, in particular to using a Raney nickel catalyst to efficiently catalyze the addition of 3-nitro-4-methoxyacetanilide The invention relates to the highly selective preparation of 3-amino-4-methoxyacetanilide, which belongs to the technical field of fine chemicals. Background technique [0002] 3-Amino-4-methoxyacetanilide is an important intermediate for the preparation of C.I. Disperse Blue 79 and Disperse Violet 58 series of disperse dyes. 3-Amino-4-methoxyacetanilide is a disperse dye used as a coupling component, which has the advantages of stable quality, high emission intensity, and excellent application performance. At present, the demand at home and abroad is very huge. [0003] Research at home and abroad shows that there are mainly two methods for synthesizing 3-amino-4-methoxyacetanilide. One is to use 2,4-dinitrochlorobenzene as ra...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
IPC IPC(8): C07C233/43C07C231/12B01J25/02
Inventor 沈灵沁殷恒波颜晓波王爱丽廖喜慧曹建翠
Owner JIANGSU UNIV
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap