CN101157633A - Method for preparing 4-bromine phenylhydrazine - Google Patents
Method for preparing 4-bromine phenylhydrazine Download PDFInfo
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- CN101157633A CN101157633A CNA2007101354728A CN200710135472A CN101157633A CN 101157633 A CN101157633 A CN 101157633A CN A2007101354728 A CNA2007101354728 A CN A2007101354728A CN 200710135472 A CN200710135472 A CN 200710135472A CN 101157633 A CN101157633 A CN 101157633A
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- bromophenyl
- hydrazine
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Abstract
The invention relates to a preparation method of 4-bromophenylhydrazine. By using 4-bromaniline as the initial raw material, the preparation method is capable of producing the 4-bromophenylhydrazine after the diazotization reaction, the reduction reaction and hydrolysis, wherein, the reduction reaction which utilizes sodium metabisulfite as the reduction agent is carried out under the conditions that the temperature is 10 to 35 DEG C and the PH value is 7 to 9. The 4-bromophenylhydrazine produced by the preparation method of the invention has the advantages of high product purity and low production cost.
Description
Technical field
The present invention relates to a kind of preparation method of 4-bromophenyl-hydrazine.
Background technology
The 4-bromophenyl-hydrazine is a kind of important intermediate, especially a kind of medicine intermediate, prior art is a raw material with the 4-bromaniline, through diazotization reaction, S-WAT reduction, hydrolysis, the synthetic method of the 4-bromophenyl-hydrazine 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 4-bromophenyl-hydrazine, the 4-bromophenyl-hydrazine 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 4-bromophenyl-hydrazine is a starting raw material with the 4-bromaniline, through diazotization reaction, and reduction reaction, hydrolysis prepares the 4-bromophenyl-hydrazine, and 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, production cost is low, and the product purity height (greater than 98%) that makes.
Embodiment
Below the specific embodiment of the present invention is described:
In the 600ml beaker, add entry 100ml, 10N hydrochloric acid 57.5ml stirs, and adds 4-bromaniline 34.6 grams, heat and make it all slowly solution to be cooled to 0 ℃ after the dissolving to 40 ℃, slowly add sodium nitrite solution (being made into by 15 gram Sodium Nitrites and 30ml water), finish, regulation system pH is 1-2,7 ℃ of the temperature of control reaction system, react after 30 minutes, stopped reaction filters and reservation filtrate.
Add entry 125ml in the 1000ml beaker, stir adding Sodium Pyrosulfite 64 grams, sodium hydroxide 65 grams down, this moment, pH value of solution was 7, solution temperature is 35 ℃, treat that solution is cooled to 20 ℃ after, slowly above-mentioned filtrate is added, the control solution temperature is 20 ℃, and pH is 7, continues reaction 30 minutes, the reaction system to 80 of heating ℃ stirs, and adds hydrochloric acid 115ml, continue to heat to 97-100 ℃, and in reaction under this temperature after 0.5 hour, cooling system to 20 ℃ is filtered and is kept filter cake.
Add water 170ml in the 300ml beaker, hydrochloric acid 11.5ml stirs, and adds above-mentioned filter cake, heats to 95-97 ℃, adds gac 2 grams, and after-filtration got filtrate in 5 minutes.Add hydrochloric acid 18.4 grams in filtrate, material is separated out, and is cooled to 10-15 ℃ of filtration, the dry product that gets.It is 98.56% that high performance liquid chromatography detects its purity.
Claims (2)
1. the preparation method of a 4-bromophenyl-hydrazine is a starting raw material with the 4-bromaniline, through diazotization reaction, reduction reaction, hydrolysis prepares the 4-bromophenyl-hydrazine, 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 4-bromophenyl-hydrazine 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 |
|---|---|---|---|
| CNA2007101354728A CN101157633A (en) | 2007-11-12 | 2007-11-12 | Method for preparing 4-bromine phenylhydrazine |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007101354728A CN101157633A (en) | 2007-11-12 | 2007-11-12 | Method for preparing 4-bromine phenylhydrazine |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101157633A true CN101157633A (en) | 2008-04-09 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2007101354728A Pending CN101157633A (en) | 2007-11-12 | 2007-11-12 | Method for preparing 4-bromine phenylhydrazine |
Country Status (1)
| Country | Link |
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| CN (1) | CN101157633A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106565534A (en) * | 2016-10-28 | 2017-04-19 | 浙江奇彩环境科技股份有限公司 | Synthesis method for aromatic hydrazine sulfate |
-
2007
- 2007-11-12 CN CNA2007101354728A patent/CN101157633A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106565534A (en) * | 2016-10-28 | 2017-04-19 | 浙江奇彩环境科技股份有限公司 | Synthesis method for aromatic hydrazine sulfate |
| CN106565534B (en) * | 2016-10-28 | 2018-10-30 | 浙江奇彩环境科技股份有限公司 | A kind of synthetic method of aryl hydrazine sulfate |
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| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C12 | Rejection of a patent application after its publication | ||
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Open date: 20080409 |