CN102358944A - Preparation method of aminopyridine chloride - Google Patents
Preparation method of aminopyridine chloride Download PDFInfo
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- CN102358944A CN102358944A CN2011102433545A CN201110243354A CN102358944A CN 102358944 A CN102358944 A CN 102358944A CN 2011102433545 A CN2011102433545 A CN 2011102433545A CN 201110243354 A CN201110243354 A CN 201110243354A CN 102358944 A CN102358944 A CN 102358944A
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Abstract
The invention discloses a preparation method of an aminopyridine chloride, relating to the field of preparation of the aminopyridine chloride and aiming to solve the problems of low product yield, more byproducts in products, complex operation process and serious environment pollution in the traditional aminopyridine synthesis process. The preparation method comprises the following steps of: 1, electrolyzing, and 2, separating and purifying. The preparation method disclosed by the invention has the advantage of: 1, very high selectivity, fewer byproducts in the products, high product purity and simplicity for postprocessing; 2, simplicity for operation, no need of any catalysts, mild reaction conditions and low energy consumption; 3, reduced consumed energy for reaction due to adoption of a diaphragm-free electrolytic cell; 4, capability of meeting requirements of green chemistry for environment friendliness; and 5, production safety. The preparation method disclosed by the invention is mainly used for preparing 2-amino-5-chloropyridine and 3-amino-2-chloropyridine.
Description
Technical field
The present invention relates to the muriatic preparation field of EL-970.
Background technology
The EL-970 muriate is important medicine and pesticide intermediate, is mainly used in important chemical products such as synthetic medicine, agricultural chemicals, dyestuff.Like 3-amino-2-chloropyridine and verivate thereof is one type of very useful EL-970 analog derivative; It can be used to the medicine-pirenzepine of synthetic treatment digestive system as important medicine intermediate; Pirenzepine is a kind of good anti-ulcerative drug, is mainly used in the treatment of gastric and duodenal ulcer.By amino-2 chloropyridines of the 3-synthetic 2 that sets out, the 3-dichloropyridine is the important intermediate of synthetic anthranilamide-based agricultural chemical insecticide (like the chlorine insect amide and the cyanogen insect amide of E.I.Du Pont Company's exploitation).Other EL-970 muriates can be used for preparing the important intermediate of medicines such as anodyne, antiphlogistic drug.Therefore the research of EL-970 muriate synthetic is significant, and prospect is very wide.At present, the muriatic compound method of the EL-970 of bibliographical information is following:
(1) EL-970 is at FeCl
3Exist down Deng Lewis acid, obtain the corresponding chlorinated EL-970 with the chlorine direct chlorination.For example: the chlorination of 2-EL-970 obtains 2-amino-5-chloropyridine, and a certain amount of 2-amino-3-chloropyridine and 2-amino-3 is arranged simultaneously, and 5-dichloropyridine by product generates; 3-EL-970 chlorination principal product is 3-amino-2-chloropyridine, and by product is 3-amino-6-chloropyridine and 3-amino-2, the 6-dichloropyridine.This method is one of technology commonly used in the industrial production, and the principal product yield is generally 60-80%.But the direct chlorination method uses chlorine to make chlorination reagent, and processing condition control is complicated, the tail gas recycle difficulty, and equipment corrosion and environmental pollution are serious.In addition, by product is more and separation difficulty also is one of shortcoming of direct chlorination method.
(2) EL-970 is dissolved in the mixed solution of hydrochloric acid and ydrogen peroxide 50 the Cl that hydrochloric acid and ydrogen peroxide 50 reaction generate
2Generate the corresponding chlorinated EL-970 with the EL-970 reaction.For example, the chlorination of 3-EL-970 obtains 3-amino-2-chloropyridine and by product 3-amino-2, the 6-dichloropyridine, and principal product 3-amino-2-chloropyridine yield can reach about 70%.The advantage of this method is not use chlorine, has avoided equipment corrosion and problem of environmental pollution because of using chlorine to bring.In addition, this chlorination reaction need not used catalyzer, has reduced production cost, has simplified purifying products technology, is a kind of chlorination method that development potentiality is arranged very much.The main drawback of present method is that the amount of by product is bigger, is generally 20～30%, has increased the difficulty of separation of by-products.
Except that above-mentioned method with the synthesizing chlorinated EL-970 of EL-970 direct chlorination; Also have some to come the report of synthesizing chlorinated EL-970 through the method for functional group's conversion; For example: with the 2-EL-970 is raw material; Through nitrated, prepared in reaction such as acidylate, reduction, chloro and hydrolysis 2-amino-5-chloropyridine.This method productive rate has only about 50%, does not also reach the degree of industrial applications at present; With 2-chloro-3-cyanopyridine is raw material, and hydrolysis prepares 2-chloro-3-acid amides pyridine under alkaline condition, carries out Hofmann degradation then, obtains the finished product, yield about 65%.
Know that through above-mentioned the product yield that exists in the existing EL-970 synthesis technique is low, by product is many in the product, operating procedure is complicated and cause serious environmental pollution problems.
Summary of the invention
The present invention will solve that the product yield that exists in the existing EL-970 synthesis technique is low, by product is many in the product, operating procedure is complicated and cause serious environmental pollution problems, and provides a kind of EL-970 muriatic preparation method.
The muriatic preparation method of a kind of EL-970, specifically accomplish according to the following steps:
One, electrolysis: EL-970 is dissolved in the hydrochloric acid soln of diaphragmless cell; Obtain EL-970 and dissolve electrolytic solution, energized feeds nitrogen simultaneously above diaphragmless cell then; Adjusting strength of current is 0.1A～0.4A; Voltage is 1.1V～1.4V, and electrolytic chlorination 2～12h at room temperature obtains the reaction solution after the electrolysis; Two, separate purification: add alkaline matter in the reaction solution after the step 1 electrolysis pH value is adjusted between 8～9; Adopt organic solvent extraction then; The separating and extracting phase, adopting massfraction is 15%～35% sodium chloride solution washing extraction phase, to the pH value of extraction phase be 7～7.5; Using vacuum distillation method to remove the pH value at last is the organic solvent in 7～7.5 extraction phases, can obtain the EL-970 muriate; EL-970 described in the step 1 is 2-EL-970 or 3-EL-970; The massfraction of HCl is 10～36% in the hydrochloric acid soln described in the step 1; Quality-volumetric concentration that EL-970 described in the step 1 dissolves EL-970 in the electrolytic solution is 15～35g/L; Alkaline matter described in the step 2 is sodium hydroxide, Pottasium Hydroxide, yellow soda ash, salt of wormwood, sodium hydrogencarbonate or saleratus; Organic solvent described in the step 2 is ETHYLE ACETATE, ether, methylene dichloride, ethylene dichloride, trichloromethane or toluene.
Advantage of the present invention: one, the present invention adopts the electrolytic chlorination method to prepare the EL-970 muriate to have very high selectivity; The 2-EL-970 is 80%～94% for the yield that the raw material electrolytic chlorination obtains principal product 2-amino-5-chloropyridine; With the 3-EL-970 is that the yield that raw material obtains principal product 3-amino-2-chloropyridine is 75%～92%; And by product is few in the product, and product purity is high, and aftertreatment is simple; Two, the present invention adopts the electrolytic chlorination method, and is simple to operate, can accomplish at ambient temperature, and reaction process need not heating, need not any catalyzer, and reaction conditions is gentle, and energy consumption is low; Three, the present invention adopts diaphragmless cell, and is lower than the required electrolysis voltage of diaphragm type electrolyzer, reduced the energy consumption of reaction; Four, the nascent state Cl that utilizes electrolysis hydrochloric acid to produce among the present invention
2EL-970 is carried out the synthesizing chlorinated EL-970 of original position chlorination reaction, avoid the use of chlorine and make caused equipment corrosion of chlorination reagent and problem of environmental pollution, meet eco-friendly Green Chemistry requirement; Five, the present invention reaches control electrolytic chlorination speed of response through the method for control current size, reduces Cl
2Overflow, improved current efficiency, and when electrolytic chlorination, above electrolyzer, fed the H that the nitrogen dilution reaction produces
2With a spot of Cl
2, guarantee production safety;
Description of drawings
Fig. 1 is that practical implementation is the nmr spectrum of the EL-970 muriate employing 1H NMR test analysis of mode nine preparations.Fig. 2 is that practical implementation is the nmr spectrum of the EL-970 muriate employing 1H NMR test analysis of mode 14 preparations.
Embodiment
Embodiment one: the muriatic preparation method of a kind of EL-970 of this embodiment, specifically accomplish according to the following steps:
One, electrolysis: EL-970 is dissolved in the hydrochloric acid soln of diaphragmless cell; Obtain EL-970 and dissolve electrolytic solution, energized feeds nitrogen simultaneously above diaphragmless cell then; Adjusting strength of current is 0.1A～0.4A; Voltage is 1.1V～1.4V, and electrolytic chlorination 2～12h at room temperature obtains the reaction solution after the electrolysis; Two, separate purification: add alkaline matter in the reaction solution after the step 1 electrolysis pH value is adjusted between 8～9; Adopt organic solvent extraction then; The separating and extracting phase, adopting massfraction is 15%～35% sodium chloride solution washing extraction phase, to the pH value of extraction phase be 7～7.5; Using vacuum distillation method to remove the pH value at last is the organic solvent in 7～7.5 extraction phases, can obtain the EL-970 muriate;
EL-970 described in this embodiment step 1 is 2-EL-970 or 3-EL-970; The massfraction of HCl is 10～36% in the hydrochloric acid soln described in this embodiment step 1; The mass concentration that EL-970 described in this embodiment step 1 dissolves EL-970 in the electrolytic solution is 15～35g/L.
Alkaline matter described in this embodiment step 2 is sodium hydroxide, Pottasium Hydroxide, yellow soda ash, salt of wormwood, sodium hydrogencarbonate or saleratus; Organic solvent described in this embodiment step 2 is ETHYLE ACETATE, ether, methylene dichloride, ethylene dichloride, trichloromethane or toluene.
The nascent state Cl that this embodiment produces with electrolysis hydrochloric acid
2With EL-970 generation original position chlorination reaction, its principle is following:
Cathodic area:
Positive column:
This embodiment employing electrolytic chlorination method prepares the EL-970 muriate and has very high selectivity; The 2-EL-970 is that principal product is 2-amino-5-chloropyridine for the raw material electrolytic chlorination obtains the EL-970 muriate, and yield is 80%～94%, is that to obtain EL-970 muriate principal product be 3-amino-2-chloropyridine to raw material with the 3-EL-970; Yield is 75%～92%; And by product is few in the product, and product purity is high, and aftertreatment is simple.
This embodiment adopts the electrolytic chlorination method, and is simple to operate, can accomplish at ambient temperature, and reaction process need not heating, need not any catalyzer, and reaction conditions is gentle, and energy consumption is low.
This embodiment adopts diaphragmless cell, and is lower than the required electrolysis voltage of diaphragm type electrolyzer, reduced the energy consumption of reaction.
The nascent state Cl that utilizes electrolysis hydrochloric acid to produce in this embodiment
2EL-970 is carried out original position chlorination reaction synthesizing amino pyridinium chloride, avoid the use of chlorine and make caused equipment corrosion of chlorination reagent and problem of environmental pollution, meet eco-friendly Green Chemistry requirement.
This embodiment reaches control electrolytic chlorination speed of response through the method for control current size, reduces Cl
2Overflow, improved current efficiency, and when electrolytic chlorination, above electrolyzer, fed the H that the nitrogen dilution reaction produces
2With a spot of Cl
2, guarantee production safety.
Embodiment two: this embodiment with the difference of embodiment one is: the massfraction of HCl is 15～30% in the hydrochloric acid soln described in the step 1.Other is identical with embodiment one.
Embodiment three: this embodiment with one of embodiment one or two difference is: the massfraction of HCl is 20% in the hydrochloric acid soln described in the step 1.Other is identical with embodiment one or two.
Embodiment four: this embodiment with one of embodiment one to three difference is: the mass concentration that the EL-970 described in the step 1 dissolves EL-970 in the electrolytic solution is 20～30g/L.Other is identical with embodiment one to three.
Embodiment five: this embodiment with one of embodiment one to four difference is: the mass concentration that the EL-970 described in the step 1 dissolves EL-970 in the electrolytic solution is 25g/L.Other is identical with embodiment one to four.
Embodiment six: this embodiment with one of embodiment one to five difference is: the employing massfraction is 20%～30% sodium chloride solution washing extraction phase in the step 2.Other is identical with embodiment one to five.
Embodiment seven: this embodiment with one of embodiment one to six difference is: the employing massfraction is 26% sodium chloride solution washing extraction phase in the step 2.Other and embodiment one to six phase are together.
Embodiment eight: this embodiment with one of embodiment one to seven difference is: the muriatic preparation method of a kind of EL-970 accomplishes according to the following steps:
One, electrolysis: the 2-EL-970 is dissolved in the hydrochloric acid soln of diaphragmless cell, obtains EL-970 and dissolve electrolytic solution, energized then; Simultaneously above electrolyzer, feed nitrogen, adjusting strength of current is 0.1A, and voltage is 1.1V; Electrolytic chlorination 4h at room temperature obtains the reaction solution after the electrolysis; Two, separate purification: add NaOH in the reaction solution after the step 1 electrolysis pH value is adjusted between 8.5; Adopt ethyl acetate extraction then; The separating and extracting phase, adopting massfraction is 26% sodium chloride solution washing extraction phase, to the pH value of extraction phase be 7; Using vacuum distillation method to remove the pH value at last is the ETHYLE ACETATE in 7 extraction phases, can obtain the EL-970 muriate.
The massfraction of HCl is 20% in the hydrochloric acid soln described in this embodiment step 1; The mass concentration that EL-970 described in this embodiment step 1 dissolves 2-EL-970 in the electrolytic solution is 25g/L.
Through the EL-970 muriate of this embodiment of gas chromatographic analysis preparation, can know that principal product is 2-amino-5-chloropyridine, yield is 79%, and by product is 2-amino-3-chloropyridine, and yield is 21%.
Embodiment nine: this embodiment with one of embodiment one to seven difference is: the muriatic preparation method of a kind of EL-970 accomplishes according to the following steps:
One, electrolysis: the 2-EL-970 is dissolved in the hydrochloric acid soln of diaphragmless cell; Obtain EL-970 and dissolve electrolytic solution, energized feeds nitrogen simultaneously above electrolyzer then; Adjusting strength of current is 0.2A; Voltage is 1.2V, and electrolytic chlorination 3.5h at room temperature obtains the reaction solution after the electrolysis; Two, separate purification: add NaOH in the reaction solution after the step 1 electrolysis pH value is adjusted between 8.5; Adopt ethyl acetate extraction then; The separating and extracting phase, adopting massfraction is 26% sodium chloride solution washing extraction phase, to the pH value of extraction phase be 7; Using vacuum distillation method to remove the pH value at last is the ETHYLE ACETATE in 7 extraction phases, can obtain the EL-970 muriate.
The massfraction of HCl is 20% in the hydrochloric acid soln described in this embodiment step 1; The mass concentration that EL-970 described in this embodiment step 1 dissolves 2-EL-970 in the electrolytic solution is 25g/L.
Through the EL-970 muriate of this embodiment of gas chromatographic analysis preparation, can know that principal product is 2-amino-5-chloropyridine, yield is 94%, and by product is 2-amino-3-chloropyridine, and yield is 6%.
Product to the preparation of this embodiment adopts 1H NMR test analysis; As shown in Figure 1, through Fig. 1 can know that electrolytic chlorination obtains principal product 2-amino-5-chloropyridine molecular structural formula is
Embodiment ten: this embodiment with one of embodiment one to seven difference is: the muriatic preparation method of a kind of EL-970 accomplishes according to the following steps:
One, electrolysis: the 2-EL-970 is dissolved in the hydrochloric acid soln of diaphragmless cell; Obtain EL-970 and dissolve electrolytic solution, energized feeds nitrogen simultaneously above electrolyzer then; Adjusting strength of current is 0.3A; Voltage is 1.3V, and electrolytic chlorination 170min at room temperature obtains the reaction solution after the electrolysis; Two, separate purification: add NaOH in the reaction solution after the step 1 electrolysis pH value is adjusted between 8.5; Adopt ethyl acetate extraction then; The separating and extracting phase, adopting massfraction is 26% sodium chloride solution washing extraction phase, to the pH value of extraction phase be 7; Using vacuum distillation method to remove the pH value at last is the ETHYLE ACETATE in 7 extraction phases, can obtain the EL-970 muriate.
The massfraction of HCl is 20% in the hydrochloric acid soln described in this embodiment step 1; The mass concentration that EL-970 described in this embodiment step 1 dissolves 2-EL-970 in the electrolytic solution is 25g/L.
Through the EL-970 muriate of this embodiment of gas chromatographic analysis preparation, can know that principal product is 2-amino-5-chloropyridine, yield is 90%, and by product is 2-amino-3-chloropyridine, and yield is 10%.
Embodiment 11: this embodiment with one of embodiment one to seven difference is: the muriatic preparation method of a kind of EL-970 accomplishes according to the following steps:
One, electrolysis: the 2-EL-970 is dissolved in the hydrochloric acid soln of diaphragmless cell; Obtain EL-970 and dissolve electrolytic solution, energized feeds nitrogen simultaneously above electrolyzer then; Adjusting strength of current is 0.4A; Voltage is 1.4V, and electrolytic chlorination 130min at room temperature obtains the reaction solution after the electrolysis; Two, separate purification: add NaOH in the reaction solution after the step 1 electrolysis pH value is adjusted between 8.5; Adopt ethyl acetate extraction then; The separating and extracting phase, adopting massfraction is 26% sodium chloride solution washing extraction phase, to the pH value of extraction phase be 7; Using vacuum distillation method to remove the pH value at last is the ETHYLE ACETATE in 7 extraction phases, can obtain this EL-970 muriate.
The massfraction of HCl is 20% in the hydrochloric acid soln described in this embodiment step 1; The mass concentration that EL-970 described in this embodiment step 1 dissolves 2-EL-970 in the electrolytic solution is 25g/L.
Through the EL-970 muriate of this embodiment of gas chromatographic analysis preparation, can know that principal product is 2-amino-5-chloropyridine, yield is 86%, and by product is 2-amino-3-chloropyridine, and yield is 14%.
Embodiment 12: this embodiment with one of embodiment one to seven difference is: the muriatic preparation method of a kind of EL-970 accomplishes according to the following steps:
One, electrolysis: the 3-EL-970 is dissolved in the hydrochloric acid soln of diaphragmless cell, obtains EL-970 and dissolve electrolytic solution, energized then; Simultaneously above electrolyzer, feed nitrogen, adjusting strength of current is 0.1A, and voltage is 1.1V; Electrolytic chlorination 4h at room temperature obtains the reaction solution after the electrolysis; Two, separate purification: add NaOH in the reaction solution after the step 1 electrolysis pH value is adjusted between 8.5; Adopt ethyl acetate extraction then; The separating and extracting phase, adopting massfraction is 26% sodium chloride solution washing extraction phase, to the pH value of extraction phase be 7; Using vacuum distillation method to remove the pH value at last is the ETHYLE ACETATE in 7 extraction phases, can obtain the EL-970 muriate.
The massfraction of HCl is 20% in the hydrochloric acid soln described in this embodiment step 1; The mass concentration that EL-970 described in this embodiment step 1 dissolves 3-EL-970 in the electrolytic solution is 25g/L.
Through the EL-970 muriate of this embodiment of gas chromatographic analysis preparation, can know that principal product is 3-amino-2-chloropyridine, yield is 72%, and by product is a 3-amino-2, and 6-chloropyridine, yield are 28%.
Embodiment 13: this embodiment with one of embodiment one to seven difference is: the muriatic preparation method of a kind of EL-970 accomplishes according to the following steps:
One, electrolysis: the 3-EL-970 is dissolved in the hydrochloric acid soln of diaphragmless cell; Obtain EL-970 and dissolve electrolytic solution, energized feeds nitrogen simultaneously above electrolyzer then; Adjusting strength of current is 0.2A; Voltage is 1.2V, and electrolytic chlorination 3.5h at room temperature obtains the reaction solution after the electrolysis; Two, separate purification: add NaOH in the reaction solution after the step 1 electrolysis pH value is adjusted between 8.5; Adopt ethyl acetate extraction then; The separating and extracting phase, adopting massfraction is 26% sodium chloride solution washing extraction phase, to the pH value of extraction phase be 7; Using vacuum distillation method to remove the pH value at last is the ETHYLE ACETATE in 7 extraction phases, can obtain the EL-970 muriate.
The massfraction of HCl is 20% in the hydrochloric acid soln described in this embodiment step 1; The mass concentration that EL-970 described in this embodiment step 1 dissolves 3-EL-970 in the electrolytic solution is 25g/L.
Through the EL-970 muriate of this embodiment of gas chromatographic analysis preparation, can know that principal product is 3-amino-2-chloropyridine, yield is 83%, and by product is a 3-amino-2, and 6-chloropyridine, yield are 17%.
Embodiment 14: this embodiment with one of embodiment one to seven difference is: the muriatic preparation method of a kind of EL-970 accomplishes according to the following steps:
One, electrolysis: the 3-EL-970 is dissolved in the hydrochloric acid soln of diaphragmless cell; Obtain EL-970 and dissolve electrolytic solution, energized feeds nitrogen simultaneously above electrolyzer then; Adjusting strength of current is 0.3A; Voltage is 1.3V, and electrolytic chlorination 170min at room temperature obtains the reaction solution after the electrolysis; Two, separate purification: add NaOH in the reaction solution after the step 1 electrolysis pH value is adjusted between 8.5; Adopt ethyl acetate extraction then; The separating and extracting phase, adopting massfraction is 26% sodium chloride solution washing extraction phase, to the pH value of extraction phase be 7; Using vacuum distillation method to remove the pH value at last is the ETHYLE ACETATE in 7 extraction phases, can obtain the EL-970 muriate.
The massfraction of HCl is 20% in the hydrochloric acid soln described in this embodiment step 1; The mass concentration that EL-970 described in this embodiment step 1 dissolves 3-EL-970 in the electrolytic solution is 25g/L.
Through the EL-970 muriate of this embodiment of gas chromatographic analysis preparation, can know that principal product is 3-amino-2-chloropyridine, yield is 89%, and by product is a 3-amino-2, and 6-chloropyridine, yield are 11%.
Product to the preparation of this embodiment adopts 1H NMR test analysis; As shown in Figure 2, through Fig. 2 can know that electrolytic chlorination obtains principal product 3-amino-2-chloropyridine molecular structural formula is
Embodiment 15: this embodiment with one of embodiment one to seven difference is: the muriatic preparation method of a kind of EL-970 accomplishes according to the following steps:
One, electrolysis: the 3-EL-970 is dissolved in the hydrochloric acid soln of diaphragmless cell; Obtain EL-970 and dissolve electrolytic solution, energized feeds nitrogen simultaneously above electrolyzer then; Adjusting strength of current is 0.4A; Voltage is 1.4V, and electrolytic chlorination 130min at room temperature obtains the reaction solution after the electrolysis; Two, separate purification: add NaOH in the reaction solution after the step 1 electrolysis pH value is adjusted between 8.5; Adopt ethyl acetate extraction then; The separating and extracting phase, adopting massfraction is 26% sodium chloride solution washing extraction phase, to the pH value of extraction phase be 7; Using vacuum distillation method to remove the pH value at last is the ETHYLE ACETATE in 7 extraction phases, can obtain the EL-970 muriate.
The massfraction of HCl is 20% in the hydrochloric acid soln described in this embodiment step 1; The mass concentration that EL-970 described in this embodiment step 1 dissolves 3-EL-970 in the electrolytic solution is 25g/L.
Through the EL-970 muriate of this embodiment of gas chromatographic analysis preparation, can know that principal product is 3-amino-2-chloropyridine, yield is 79%, and by product is a 3-amino-2, and 6-chloropyridine, yield are 21%.
Claims (4)
1. muriatic preparation method of EL-970 is characterized in that the muriatic preparation method of EL-970 accomplishes according to the following steps:
One, electrolysis: EL-970 is dissolved in the hydrochloric acid soln of diaphragmless cell; Obtain EL-970 and dissolve electrolytic solution, energized feeds nitrogen simultaneously above diaphragmless cell then; Adjusting strength of current is 0.1A～0.4A; Voltage is 1.1V～1.4V, and electrolytic chlorination 2～12h at room temperature obtains the reaction solution after the electrolysis; Two, separate purification: add alkaline matter in the reaction solution after the step 1 electrolysis pH value is adjusted between 8～9; Adopt organic solvent extraction then; The separating and extracting phase, adopting massfraction is 15%～35% sodium chloride solution washing extraction phase, to the pH value of extraction phase be 7～7.5; Using vacuum distillation method to remove the pH value at last is the organic solvent in 7～7.5 extraction phases, can obtain the EL-970 muriate; EL-970 described in the step 1 is 2-EL-970 or 3-EL-970; The massfraction of HCl is 10～36% in the hydrochloric acid soln described in the step 1; Quality-volumetric concentration that EL-970 described in the step 1 dissolves EL-970 in the electrolytic solution is 15～35g/L; Alkaline matter described in the step 2 is sodium hydroxide, Pottasium Hydroxide, yellow soda ash, salt of wormwood, sodium hydrogencarbonate or saleratus; Organic solvent described in the step 2 is ETHYLE ACETATE, ether, methylene dichloride, ethylene dichloride, trichloromethane or toluene.
2. the muriatic preparation method of a kind of EL-970 according to claim 1, the massfraction that it is characterized in that HCl in the hydrochloric acid soln described in the step 1 is 15～30%.
3. the muriatic preparation method of a kind of EL-970 according to claim 2 is characterized in that the mass concentration of EL-970 in the molten electrolytic solution of the EL-970 described in the step 1 is 20～30g/L.
4. according to claim 1, the muriatic preparation method of 2 or 3 described a kind of EL-970s, it is characterized in that adopting in the step 2 massfraction is 20%～30% sodium chloride solution washing extraction phase.
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| CN103556174A (en) * | 2013-10-21 | 2014-02-05 | 哈尔滨理工大学 | Synthesis method of ethyl 4-chloro-1-methyl-3-ethyl-5-pyrazolylcarboxylate |
| CN106432069A (en) * | 2016-09-09 | 2017-02-22 | 安徽工业大学 | A method for preparation of 2-amino-5-chloro-pyridine |
| CN112410808A (en) * | 2020-10-04 | 2021-02-26 | 浙江埃森化学有限公司 | Synthesis method of anthranilate pesticide containing N-pyridylpyrazole |
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| CN106432069A (en) * | 2016-09-09 | 2017-02-22 | 安徽工业大学 | A method for preparation of 2-amino-5-chloro-pyridine |
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