CN102603638A - Synthesis process of pyrazole amine - Google Patents
Synthesis process of pyrazole amine Download PDFInfo
- Publication number
- CN102603638A CN102603638A CN2012100362732A CN201210036273A CN102603638A CN 102603638 A CN102603638 A CN 102603638A CN 2012100362732 A CN2012100362732 A CN 2012100362732A CN 201210036273 A CN201210036273 A CN 201210036273A CN 102603638 A CN102603638 A CN 102603638A
- Authority
- CN
- China
- Prior art keywords
- methyl hydrazine
- synthesis technique
- toluene
- pyrazoles
- aqueous solution
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Abstract
The invention relates to an intermediate for producing medicines and pesticides, in particular to a synthesis process of pyrazole amine, belonging to the technical field of chemistry. The synthesis process uses 40% methyl hydrazine aqueous solution and ethoxy methylene ethyl cyanoacetate as raw materials, and toluene is adopted as a solvent, wherein the 40% methyl hydrazine aqueous solution is available, and the danger of the 40% methyl hydrazine aqueous solution to human body is small, the safety is high, and the cost is low. As the toluene is taken as the solvent, the process is simple, and the operation is easy, the reaction time is greatly shortened, the product yield is high, and none of the three wastes is discharged.
Description
Technical field
The present invention relates to a kind of production medicine, pesticide intermediate, be specifically related to a kind of pyrazoles amine synthesis technique, belong to technical field of chemistry.
Background technology
Pyrazoles amine is medicine and a kind of important intermediate of agricultural chemicals, and the technology of producing this kind product in the market all adopts 99.9% methyl hydrazine to make raw material, makes solvent with alcohol.The problem that this kind technology exists is: 1,99.9% methyl hydrazine is inflammable, explosive, poor stability, and cost an arm and a leg, market supply is not enough.2, make solvent with alcohol, troublesome poeration.3, this technological reaction time long, above 24 hours.Poor stability, yield is low, can only reach 70% yield, and cost is high.
Summary of the invention
The objective of the invention is to overcome the weak point of above-mentioned prior art, a kind of pyrazoles amine synthesis technique is provided.These synthesis technique starting material adopt the 40% methyl hydrazine aqueous solution, oxyethyl group methene base ethyl cyanoacetate, and solvent adopts toluene.Wherein 40% methyl hydrazine solution materials is easy to get, and little to human harm property, safe, cost is low.Adopt toluene to make solvent, technology is simple, and is easy to operate, and the reaction times shortens greatly, and product yield is high, three-waste free discharge.
The present invention realizes with following technical scheme: a kind of pyrazoles amine synthesis technique, it is characterized in that: this synthesis technique comprises the steps:
(1) oxyethyl group methene base ethyl cyanoacetate is dropped in the reaction kettle, resorb toluene after the stirring and dissolving, sucks the dropping jar with methyl hydrazine; Open chilled brine, begin to drip methyl hydrazine when dropping to 20 ℃, temperature remains on 30 ℃, drips to finish insulation 1 hour;
Its chemical equation is:
(2) drive steam valve then, slowly be raised to reflux temperature, refluxed 2 hours, open freezingly, cool to 9-10 ℃ of discharging, the filter cake oven dry is pyrazoles amine, and the toluene recovery set is used.
Described starting material adopt the 40% methyl hydrazine aqueous solution, oxyethyl group methene base ethyl cyanoacetate, and solvent adopts toluene.
Described temperature of reaction is 20 ℃, and holding temperature is 30 ℃.
The described reaction times is that soaking time is 1 hour, and return time is 2 hours.
Advantage of the present invention is: these synthesis technique starting material adopt the 40% methyl hydrazine aqueous solution, oxyethyl group methene base ethyl cyanoacetate, and solvent adopts toluene.Wherein 40% methyl hydrazine solution materials is easy to get, and little to human harm property, safe, cost is low.Adopt toluene to make solvent, technology is simple, and is easy to operate, and the reaction times shortens greatly, and product yield is high, three-waste free discharge.
Embodiment
Below in conjunction with embodiment the present invention is done further explain:
Embodiment 1,
This synthesis technique comprises the steps:
(1) oxyethyl group methene base ethyl cyanoacetate is dropped in the reaction kettle, resorb toluene after the stirring and dissolving, sucks the dropping jar with methyl hydrazine; Open chilled brine, begin to drip methyl hydrazine when dropping to 20 ℃, temperature remains on 30 ℃, drips to finish insulation 1 hour;
Its chemical equation is:
(2) drive steam valve then, slowly be raised to reflux temperature, refluxed 2 hours, open freezingly, cool to 9-10 ℃ of discharging, the filter cake oven dry is pyrazoles amine, and the toluene recovery set is used.
Described starting material adopt the 40% methyl hydrazine aqueous solution, oxyethyl group methene base ethyl cyanoacetate, and solvent adopts toluene.
Described temperature of reaction is 20 ℃, and holding temperature is 30 ℃.
The described reaction times is that soaking time is 1 hour, and return time is 2 hours.
Embodiment 2,
Whether monitoring device is in stand-by state, reaches in the power supply normal negative pressure-prepare to feed intake under 0.09Mpa and the anhydrous situation of reactive system.
The 260kg methene is put into still No. 1, resorb 700kg toluene, open stirring and dissolving after, the 200kg methyl hydrazine suck is dripped jar; Open chilled brine, begin to drip methyl hydrazine when dropping to 20 ℃, temperature remains on 30 ℃, drips to finish insulation 1 hour.
Its chemical equation is:
Drive steam valve then, slowly be raised to reflux temperature, refluxed 2 hours, open freezingly, cool to 10 ℃ of left and right sides dischargings, the filter cake oven dry is pyrazoles amine, toluene recovery set usefulness, certified products total recovery 95%.
Claims (4)
1. pyrazoles amine synthesis technique, it is characterized in that: this synthesis technique comprises the steps:
(1) oxyethyl group methene base ethyl cyanoacetate is dropped in the reaction kettle, resorb toluene after the stirring and dissolving, sucks the dropping jar with methyl hydrazine; Open chilled brine, begin to drip methyl hydrazine when dropping to 20 ℃, temperature remains on 30 ℃, drips to finish insulation 1 hour;
Its chemical equation is:
(2) drive steam valve then, slowly be raised to reflux temperature, refluxed 2 hours, open freezingly, cool to 9-10 ℃ of discharging, the filter cake oven dry is pyrazoles amine, and the toluene recovery set is used.
2. pyrazoles amine synthesis technique according to claim 1 is characterized in that: described starting material adopt the 40% methyl hydrazine aqueous solution, oxyethyl group methene base ethyl cyanoacetate, and solvent adopts toluene.
3. pyrazoles amine synthesis technique according to claim 1 is characterized in that: described temperature of reaction is 20 ℃, and holding temperature is 30 ℃.
4. pyrazoles amine synthesis technique according to claim 1 is characterized in that: the described reaction times is that soaking time is 1 hour, and return time is 2 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012100362732A CN102603638A (en) | 2012-02-17 | 2012-02-17 | Synthesis process of pyrazole amine |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012100362732A CN102603638A (en) | 2012-02-17 | 2012-02-17 | Synthesis process of pyrazole amine |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102603638A true CN102603638A (en) | 2012-07-25 |
Family
ID=46521477
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2012100362732A Pending CN102603638A (en) | 2012-02-17 | 2012-02-17 | Synthesis process of pyrazole amine |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102603638A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106831586A (en) * | 2017-01-05 | 2017-06-13 | 天门楚天精细化工有限公司 | A kind of pyrazole amine preparation method |
| CN115433129A (en) * | 2021-06-02 | 2022-12-06 | 帕潘纳(北京)科技有限公司 | Method for preparing pyrazole compound |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3489125B2 (en) * | 1992-09-01 | 2004-01-19 | 日産化学工業株式会社 | Method for producing 4-alkoxycarbonyl-5-amino-1-methylpyrazole |
| JP2011201794A (en) * | 2010-03-24 | 2011-10-13 | Fujifilm Corp | Process for producing 5-aminopyrazole derivative and salt thereof |
-
2012
- 2012-02-17 CN CN2012100362732A patent/CN102603638A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3489125B2 (en) * | 1992-09-01 | 2004-01-19 | 日産化学工業株式会社 | Method for producing 4-alkoxycarbonyl-5-amino-1-methylpyrazole |
| JP2011201794A (en) * | 2010-03-24 | 2011-10-13 | Fujifilm Corp | Process for producing 5-aminopyrazole derivative and salt thereof |
Non-Patent Citations (1)
| Title |
|---|
| 王宝玉等: "吡嘧磺隆的合成", 《延边大学学报（自然科学版）》, vol. 28, no. 3, 30 September 2002 (2002-09-30) * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106831586A (en) * | 2017-01-05 | 2017-06-13 | 天门楚天精细化工有限公司 | A kind of pyrazole amine preparation method |
| CN115433129A (en) * | 2021-06-02 | 2022-12-06 | 帕潘纳(北京)科技有限公司 | Method for preparing pyrazole compound |
| CN115433129B (en) * | 2021-06-02 | 2023-06-20 | 帕潘纳(北京)科技有限公司 | Process for preparing pyrazoles |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN100391939C (en) | Process for preparing metformin hydrochloride | |
| CN105061355B (en) | A kind of process for purification of high-purity epalrestat | |
| CN102603638A (en) | Synthesis process of pyrazole amine | |
| CN101921211A (en) | Purification method of oxytetracycline | |
| EP2462941B1 (en) | Method and installation for extraction of plant raw material | |
| CN104911031A (en) | Extraction method for citronella oil antibacterial substances | |
| CN102154001A (en) | Method for preparing solid organic boron delayed cross-linking agent | |
| CN103145645B (en) | The preparation technology of methyl mercapto thiadiazoles | |
| CN102796189B (en) | Preparation method of protamine sulfate | |
| CN102285918A (en) | Method for producing ethoxy quinoline | |
| CN104803879A (en) | Preparation technology of methoxyfenozide | |
| CN101423231A (en) | Purification method of solid cyanamide | |
| CN102807536A (en) | Preparation method of 1-(2,3-dichlorophenyl) piperazine hydrochloride | |
| CN103880832A (en) | Preparation method of thiamethoxam | |
| AU2018101959A4 (en) | N-cyclohexyl-N'-phenyl-p-phenylenediamine production plant | |
| CN101549880A (en) | Preparation method of anti-caking strontium nitrate | |
| CN103626654B (en) | One prepares the method for 2,4-D dimethylamine salt raw pesticide | |
| CN106986864B (en) | Preparation device and preparation method of azithromycin | |
| CN202682171U (en) | Ointment production line | |
| CN105693709A (en) | Technology for producing nifuratel | |
| CN103664695A (en) | Preparation method and refining method of ethoxymethylenemalononitrile | |
| CN109836483A (en) | The process units and production method of zeins | |
| CN103910684A (en) | Preparation method of 4,6-dihydroxy-5-methoxypyrimidine sodium | |
| CN104803862A (en) | Synthetic method of ether amine flotation agent | |
| CN105646357A (en) | 5-amino-1-methyl-1H-pyrazole-4-carboxylic acid ethyl ester synthesis process |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20120725 |