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Method for preparing o-anisidine by catalytic hydrogenation

A technology for o-anisole and o-nitroanisole, which is applied in the field of catalytic hydrogenation to prepare o-anisole, can solve the problems of high energy consumption, large amount of waste liquid, low product yield and the like, and achieves low energy consumption. consumption, high product quality and high yield

Inactive Publication Date: 2012-03-28
JIANGSU KANGHENG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The iron powder reduction method produces a large amount of iron sludge, seriously pollutes the environment, and consumes a lot of energy; the alkali sulfide reduction method has disadvantages such as complex reduction routes, low product yield, and large amount of waste liquid; the electrochemical reduction method consumes too much energy

Method used

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  • Method for preparing o-anisidine by catalytic hydrogenation
  • Method for preparing o-anisidine by catalytic hydrogenation
  • Method for preparing o-anisidine by catalytic hydrogenation

Examples

Experimental program
Comparison scheme
Effect test

example 1

[0022] 76.5g (0.5mol) of o-nitroanisole, 76.5g of methanol, 2.3g of catalyst Raney-Ni (3% in W%) were added to a 1L autoclave. Control the reaction pressure at 1-1.2MPa, and the reaction temperature at 50-60°C. After 4 hours of reaction, take a sample to detect 99.5% of GC anthranil.

[0023]

example 2

[0025] Add 153g of o-nitroanisole (1.0mol), 153g of methanol, 4.6g of catalyst Raney-Ni (3% in W%) into a 1L high-pressure reactor, and after nitrogen replacement for 3 times, start to raise the temperature and introduce hydrogen to control the reaction The pressure is 1-1.2MPa, the reaction temperature is between 50-60°C, after 4 hours of reaction, a sample is taken to detect 99.4% of GC anthranil, and after recovery of methanol, 115g of light yellow liquid is obtained by rectification under reduced pressure, with a yield of 93.4% , GC99.5% was detected.

[0026]

example 3

[0028] Add 306g of o-nitroanisole (2.0mol), 306g of methanol, 10.2g of catalyst Raney-Ni (3% in W%) into a 1L high-pressure reactor, and after nitrogen replacement for 3 times, start to raise the temperature and introduce hydrogen to control the reaction The pressure is 1-1.2MPa, the reaction temperature is between 50-60°C, and after 4 hours of reaction, a sample is taken to detect 99.5% of GC anthranil, and after recovery of methanol, 236g of light yellow liquid is obtained by rectification under reduced pressure, with a yield of 99.59% , GC99.6% was detected.

[0029]

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PUM

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Abstract

The invention discloses a method for preparing o-anisidine by catalytic hydrogenation. The method comprises the following steps of: mixing o-nitroanisole, methanol and a catalyst Raney-Ni, adding the mixture into a pressure kettle, performing replacement by hydrogen, introducing the hydrogen to maintain the pressure of between 0.5 and 2MPa, heating to the temperature of between 40 and 80 DEG C, introducing the hydrogen continuously for 3 to 10 hours, recovering the methanol, separating liquid and rectifying to obtain the o-anisidine. The method has the advantages of environment friendliness, low energy consumption, high yield and high quality of products.

Description

technical field [0001] The invention relates to a method for preparing o-aminoanisole by catalytic hydrogenation. Background technique [0002] Anthranil is an important dye intermediate and pharmaceutical intermediate, which can be used to prepare azo dyes, ice dyes, naphthol AS-OL and other dyes, as well as guaiacol, anisotropy and other pharmaceuticals It can also be used to produce vanillin, which is widely used in the production of fine chemicals such as pesticides, dyes, and pharmaceuticals. [0003] At present, the production route of anthranil mainly contains the following two kinds: [0004] 1. Using o-nitrophenol as a raw material, first methylated and then reduced: [0005] [0006] 2. Using o-chloronitrobenzene as raw material, first methoxylating and then reducing: [0007] [0008] The above two routes are obtained by reducing the nitro group of o-nitroanisole. Traditional nitro reduction methods mainly include iron powder reduction method, alkali s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C217/84C07C213/02
Inventor 邱志刚雍成松
Owner JIANGSU KANGHENG CHEM
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