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P-nitroanisole synthesis method

A technology of p-nitroanisole and synthesis method, which is applied in the field of synthesis of p-nitroanisole, can solve the problems of large amount of by-products, low reaction yield, and many hydrolysis by-products, etc., so as to improve the yield , the effect of high product quality

Pending Publication Date: 2020-09-11
ZHEJIANG RUNTU INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the method for preparing p-nitroanisole is mainly to feed p-nitrochlorobenzene, methanol, and solid sodium hydroxide into the autoclave for reaction at one time. However, this method has low reaction yield and the formation of by-products The amount is large, and the high-salt and high-COD wastewater generated in the production process has not been treated with effective measures, causing serious pollution to the environment
[0004] There are a large number of literature reports at present, adopt phase-transfer catalyst method to synthesize p-nitroanisole, to overcome the disadvantages of harsh reaction conditions, many hydrolysis by-products, and large amount of waste water in the existing process, but the method is not yet mature and cannot be carried out on a large scale industrial production of

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] (1) Add 1636g of p-nitrochlorobenzene and 1200g of methanol into the autoclave, close the autoclave, slowly heat up until the p-nitrochlorobenzene is basically dissolved, start stirring and continue to heat up to 80°C, and then start to oxidize 3680mL of hydrogen Sodium methanol solution (the content of sodium hydroxide is 125g / L) is added in batches to the p-nitrochlorinated benzyl alcohol solution for reaction, the dropwise addition process is controlled as follows: add 1200mL dropwise for about 1 hour; then continue to heat up to about 85°C 1840mL was added dropwise in about 2 hours; then the temperature was raised to 90-95°C, and the remaining methanolic sodium hydroxide solution was added dropwise in about 1 hour. Finally, continue to heat up to 100-105° C. for heat preservation reaction, and reach the end of the reaction in about 6 hours.

[0026] (2) Then the reaction product obtained is filtered, and the filter cake is washed with 1200g of methanol to obtain sod...

Embodiment 1-1

[0028] (1) Take one batch of the filtrate in Example 1, raise the temperature to 65°C, control the system temperature to about 65°C, and start adding dimethyl sulfate dropwise. With the dropwise addition of dimethyl sulfate, the pH of the system gradually decreases. When the pH drops When it reaches about 9.5, add sodium bicarbonate solution dropwise at the same time to maintain the pH of the system at about 9.5, first drop 5 g of dimethyl sulfate, take a sample to check the purity, the remaining p-nitrophenol is 0.91%, and continue to add dimethyl sulfate until Sampling remaining p-nitrophenol is less than 0.3% as the end point, and a total of 8 g of dimethyl sulfate is consumed.

[0029] (2) After the reaction is over, add 9.3g of liquid caustic soda, then heat up and distill to reclaim the methanol in it. After the recovery of methanol, add 200g of clear water, stir at 65°C for half an hour, and leave to separate to get the finished p-nitroanisole. It is 99.52%, and basical...

Embodiment 1-2

[0032] (1) Take one batch of the filtrate in Example 1, raise the temperature to 65°C, control the temperature of the system at about 65°C, first adjust the pH to about 9.5 with dilute sulfuric acid, then start to add dimethyl sulfate dropwise, and add sodium bicarbonate dropwise at the same time Solution, keep the pH of the system at about 9.5, first drop 5g of dimethyl sulfate, take a sample to check the purity, the remaining p-nitrophenol is 0.71%, continue to add dimethyl sulfate until the sampling remaining p-nitrophenol is less than 0.3% as the end point , A total of 6.6 g of dimethyl sulfate was consumed.

[0033] (2) After the reaction is finished, add 8 g of liquid caustic soda, then heat up and reclaim methanol therein. After the recovery of methanol, add 200 g of clear water, stir for half an hour at 65° C., and leave to stand for stratification to obtain the finished product p-Nitroanisole, with a purity of 99.27%, basically free of p-nitrophenol, the yield is 98.1...

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PUM

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Abstract

The invention relates to a synthetic method of p-nitroanisole, which can effectively reduce the generation of by-products, avoid the refining process of the by-product p-nitrophenol and greatly improve the yield of p-nitroanisole; besides, a small amount of p-nitrophenol can be further reused in the synthetic steps of the invention in the subsequent wastewater treatment process. In addition, the p-nitroanisole obtained by the method disclosed by the invention has higher product quality.

Description

technical field [0001] The invention belongs to the technical field of synthesis of fine chemicals, and in particular relates to a synthesis method of p-nitroanisole. Background technique [0002] p-nitroanisole, also known as p-nitroanisole, is an important raw material for the synthesis of p-aminoanisole, which is an important intermediate for the synthesis of dyes. When used as dyes and pharmaceutical intermediates, it is mainly used to produce dyes such as p-aminoanisole, blue salt VB, maroon base GP, and naphthol AS. [0003] At present, the method for preparing p-nitroanisole is mainly to feed p-nitrochlorobenzene, methanol, and solid sodium hydroxide into the autoclave for reaction at one time. However, this method has low reaction yield and the formation of by-products The amount is large, and the high-salt and high-COD wastewater generated in the production process has not been treated with effective measures, causing serious pollution to the environment. [0004]...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C201/12C07C201/16C07C205/37
CPCC07C201/12C07C201/16C07C205/37
Inventor 章文刚高立江赵国生和西彬
Owner ZHEJIANG RUNTU INST
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