CN101157631A - Method for preparing m-nitro phenylhydrazine - Google Patents
Method for preparing m-nitro phenylhydrazine Download PDFInfo
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- CN101157631A CN101157631A CNA2007101353937A CN200710135393A CN101157631A CN 101157631 A CN101157631 A CN 101157631A CN A2007101353937 A CNA2007101353937 A CN A2007101353937A CN 200710135393 A CN200710135393 A CN 200710135393A CN 101157631 A CN101157631 A CN 101157631A
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- phenylhydrazine
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- nitrophenyl
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Abstract
The invention relates to a preparation method for m-Nitrophenyl hydrazine. The m-Nitrophenyl hydrazine is obtained through diazotization reaction, deoxidizing reaction and hydrolysis by taking m-Nitrophenyl aniline as raw materials. The deoxidizing reaction takes sodium meta-bisulphite as the raw materials, being carried under the conditions that the temperature is 10 to 35 DEG C and the pH value is 7 to 9. The m-Nitrophenyl hydrazine produced through the method disclosed in the invention has the advantages of high purity and low production cost.
Description
Technical field
The present invention relates to a kind of preparation method of m-nitro phenylhydrazine.
Background technology
M-nitro phenylhydrazine is a kind of important intermediate, especially a kind of medicine intermediate, prior art is raw material with the m-nitraniline, through diazotization reaction, S-WAT reduction, hydrolysis, the synthetic method of the m-nitro phenylhydrazine for preparing, long reaction time generally needs yield only to be 63-72%, and the production cost height.
Summary of the invention
Technical problem to be solved by this invention provides a kind of preparation method of m-nitro phenylhydrazine, the m-nitro phenylhydrazine product purity height that obtains by this method, and production cost is low.
For solving above technical problem, the present invention adopts following technical scheme:
A kind of preparation method of m-nitro phenylhydrazine is a starting raw material with the m-nitraniline, through diazotization reaction, reduction reaction, hydrolysis prepares m-nitro phenylhydrazine, described reduction reaction is reductive agent with the Sodium Pyrosulfite, and at 10-35 ℃, pH carries out under the condition of 7-9.
The temperature of described reduction reaction is preferably 20 ℃, and pH is preferably 7.
Because the technique scheme utilization, the present invention compared with prior art has following advantage:
Adopt Sodium Pyrosulfite as reductive agent, shortened the reaction times greatly, generally only need half hour can reach reaction end, and the product purity height (greater than 98%) that makes, production cost is low.
Embodiment
Below the specific embodiment of the present invention is described:
In the 800ml beaker, add entry 110ml, stir, add 10N hydrochloric acid 126.5ml, m-nitraniline 60 grams, heating makes it all slowly solution to be cooled to 0 ℃ after the dissolving to 90 ℃, adds sodium nitrite solution (being made into by 30 gram Sodium Nitrites and 15ml water) rapidly, finish, regulation system pH is 1-2, and 5 ℃-7 ℃ of the temperature of control reaction system are reacted after 30 minutes, stopped reaction filters and reservation filtrate.
In the 2000ml beaker, add entry 250ml, stir and add Sodium Pyrosulfite 128 grams, sodium hydroxide 143 grams down, this moment, pH value of solution was 7, solution temperature is 35 ℃, after treating that solution is cooled to 18 ℃, slowly above-mentioned filtrate is added, solution temperature is 20 ℃ when adding, and pH is 7, continue reaction 30 minutes, the reaction system of heating stirs to 30-40 ℃, adds hydrochloric acid 80.5ml, continue to heat to 75-80 ℃, and adding sodium-chlor 40 grams after 1.5-2 hour in reaction under this temperature, cooling system to 20 ℃ is filtered and is kept filter cake and drying obtains product.It is 98.42% that high performance liquid chromatography is surveyed its purity.
Claims (2)
1. the preparation method of a m-nitro phenylhydrazine is a starting raw material with the m-nitraniline, through diazotization reaction, reduction reaction, hydrolysis prepares m-nitro phenylhydrazine, it is characterized in that: described reduction reaction is reductive agent with the Sodium Pyrosulfite, and at 10-35 ℃, pH carries out under the condition of 7-9.
2. the preparation method of a kind of m-nitro phenylhydrazine according to claim 1 is characterized in that: described reduction reaction is at 20 ℃, and pH carries out under 7 the condition.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007101353937A CN101157631A (en) | 2007-11-08 | 2007-11-08 | Method for preparing m-nitro phenylhydrazine |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007101353937A CN101157631A (en) | 2007-11-08 | 2007-11-08 | Method for preparing m-nitro phenylhydrazine |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101157631A true CN101157631A (en) | 2008-04-09 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2007101353937A Pending CN101157631A (en) | 2007-11-08 | 2007-11-08 | Method for preparing m-nitro phenylhydrazine |
Country Status (1)
| Country | Link |
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| CN (1) | CN101157631A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111362782A (en) * | 2020-03-16 | 2020-07-03 | 内蒙古大中实业化工有限公司 | Method for preparing m-trifluoromethylphenol |
-
2007
- 2007-11-08 CN CNA2007101353937A patent/CN101157631A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111362782A (en) * | 2020-03-16 | 2020-07-03 | 内蒙古大中实业化工有限公司 | Method for preparing m-trifluoromethylphenol |
| CN111362782B (en) * | 2020-03-16 | 2022-06-07 | 内蒙古大中实业化工有限公司 | Method for preparing m-trifluoromethylphenol |
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Open date: 20080409 |