CN109096145A - A kind of method that multi-substituent aniline prepares diazonium salt - Google Patents
A kind of method that multi-substituent aniline prepares diazonium salt Download PDFInfo
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- CN109096145A CN109096145A CN201810771358.2A CN201810771358A CN109096145A CN 109096145 A CN109096145 A CN 109096145A CN 201810771358 A CN201810771358 A CN 201810771358A CN 109096145 A CN109096145 A CN 109096145A
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- diazonium salt
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- substituent aniline
- substituent
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C245/00—Compounds containing chains of at least two nitrogen atoms with at least one nitrogen-to-nitrogen multiple bond
- C07C245/20—Diazonium compounds
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to a kind of methods that multi-substituent aniline prepares diazonium salt, a certain amount of multi-substituent aniline is weighed to be put into the reaction kettle for filling dilute hydrochloric acid, sodium fluoborate is slowly added dropwise in a kettle, make its reaction, anionic organic compounds are added in above-mentioned reaction product, mixed solution stirred crystallization, and diazonium salt filter cake is obtained by filtering, above-mentioned product is dry by drying box, and it is crushed by pulverizer, obtained product is diazonium salt, the method that a kind of multi-substituent aniline proposed by the present invention prepares diazonium salt, by using the practical sodium nitrite of sodium fluoborate substitution tradition as diazotization agent, it can effectively avoid the drawbacks of nitrous acid depression is decomposed, consequently facilitating Chemical Manufacture, simultaneously, reaction temperature can be improved as under room temperature, it may make reaction more thorough, stable diazonium salt is prepared to obtain high yield.
Description
Technical field
The invention belongs to the sides that diazonium salt production technical field more particularly to a kind of multi-substituent aniline prepare diazonium salt
Method.
Background technique
Polysubstituted primary aromatic amine is reacted with sodium nitrite in an acidic solution, and the reaction for forming diazonium salt is referred to as diazotising
Reaction, diazonium salt can be converted into a variety of fragrant substituted compounds, be widely used in organic synthesis.For nitro compound
It is poor in the dissolubility of reaction dissolvent, it is difficult to which that the deficiency that complete diazotising causes reaction that can not carry out, present invention selection are suitable
Solvent, and traditional low-temp reaction condition is changed to the controllable condition of room temperature, reaction is carried out thoroughly, and is prepared with high yield
Stable diazonium salt.
Summary of the invention
The present invention is to solve well-known technique and provide a kind of multi-substituent aniline and prepare diazonium salt
Method.
The present invention is adopted the technical scheme that solve well-known technique: a kind of multi-substituent aniline
The method for preparing diazonium salt, comprising the following steps:
A. a certain amount of multi-substituent aniline is weighed to be put into the reaction kettle for filling dilute hydrochloric acid；
B. sodium fluoborate is slowly added dropwise in a kettle, makes its reaction；
C. anionic organic compounds are added in the reaction product of step b；
D. step c mixed solution stirred crystallization, and diazonium salt filter cake is obtained by filtering；
E. step d product is dry by drying box, and crushed by pulverizer, obtained product is diazonium salt.
Preferably, the reaction kettle is stainless steel electric heating reacting kettle.
Preferably, the temperature of reaction kettle is 25-50 DEG C in the step b.
Preferably, it is filtered in the step d using screen, and is 200 mesh screens.
Preferably, the temperature of drying box is 100-200 DEG C in the step e, and drying time is 0.5-1h.
Preferably, the pulverizer in the step e is flour mill, and exit is equipped with 300 meshes.
The present invention has the advantage that as follows with good effect:
1. the method that a kind of multi-substituent aniline proposed by the present invention prepares diazonium salt is substituted by using sodium fluoborate and is passed
Practical sodium nitrite unite as diazotization agent, can effectively avoid the drawbacks of nitrous acid depression is decomposed, consequently facilitating Chemical Manufacture,
Meanwhile reaction temperature can be improved under room temperature, to may make reaction more thorough, so that obtaining high yield prepares stable diazonium
Salt.
Specific embodiment
In order to further understand the content, features and effects of the present invention, hereby enumerating following embodiment, it is described in detail such as
Under.
Embodiment 1:
The method that a kind of multi-substituent aniline of the invention prepares diazonium salt, comprising the following steps:
A. it weighs a certain amount of multi-substituent aniline to be put into the reaction kettle for filling dilute hydrochloric acid, reaction kettle is that stainless steel electricity adds
Thermal response kettle.
B. sodium fluoborate is slowly added dropwise in a kettle, makes its reaction；The temperature of reaction kettle is 35 DEG C.
C. anionic organic compounds are added in the reaction product of step b；
D. step c mixed solution stirred crystallization, and diazonium salt filter cake is obtained by filtering；It is filtered using screen, and
For 200 mesh screens.
E. step d product is dry by drying box, and crushed by pulverizer, obtained product is diazonium salt, is dried
The temperature of dry case are as follows: 150 DEG C, and drying time is 0.8h, pulverizer is flour mill, and exit is equipped with 300 meshes.
Embodiment 2:
The method that a kind of multi-substituent aniline of the invention prepares diazonium salt, comprising the following steps:
A. it weighs a certain amount of multi-substituent aniline to be put into the reaction kettle for filling dilute hydrochloric acid, reaction kettle is that stainless steel electricity adds
Thermal response kettle.
B. sodium fluoborate is slowly added dropwise in a kettle, makes its reaction；The temperature of reaction kettle is 45 DEG C.
C. anionic organic compounds are added in the reaction product of step b；
D. step c mixed solution stirred crystallization, and diazonium salt filter cake is obtained by filtering；It is filtered using screen, and
For 200 mesh screens.
E. step d product is dry by drying box, and crushed by pulverizer, obtained product is diazonium salt, is dried
The temperature of dry case are as follows: 200 DEG C, and drying time is 0.5h, pulverizer is flour mill, and exit is equipped with 300 meshes.
Above-described embodiment substitutes the practical sodium nitrite of tradition as diazotising when in use, by using sodium fluoborate
Agent can effectively avoid the drawbacks of nitrous acid depression is decomposed, consequently facilitating Chemical Manufacture, meanwhile, reaction temperature can be improved as room temperature
Under the conditions of, it may make reaction more thorough, so that obtaining high yield prepares stable diazonium salt.
The above is only the preferred embodiments of the present invention, and is not intended to limit the present invention in any form,
Any simple modification made to the above embodiment according to the technical essence of the invention, equivalent variations and modification, belong to
In the range of technical solution of the present invention.
Claims (6)
1. a kind of method that multi-substituent aniline prepares diazonium salt, which comprises the following steps:
A. a certain amount of multi-substituent aniline is weighed to be put into the reaction kettle for filling dilute hydrochloric acid；
B. sodium fluoborate is slowly added dropwise in a kettle, makes its reaction；
C. anionic organic compounds are added in the reaction product of step b；
D. step c mixed solution stirred crystallization, and diazonium salt filter cake is obtained by filtering；
E. step d product is dry by drying box, and crushed by pulverizer, obtained product is diazonium salt.
2. the method that a kind of multi-substituent aniline according to claim 1 prepares diazonium salt, which is characterized in that the reaction
Kettle is stainless steel electric heating reacting kettle.
3. the method that a kind of multi-substituent aniline according to claim 1 prepares diazonium salt, which is characterized in that the step
The temperature of reaction kettle is 25-50 DEG C in b.
4. the method that a kind of multi-substituent aniline according to claim 1 prepares diazonium salt, which is characterized in that the step
It is filtered in d using screen, and is 200 mesh screens.
5. the method that a kind of multi-substituent aniline according to claim 1 prepares diazonium salt, which is characterized in that the step
The temperature of drying box is 100-200 DEG C in e, and drying time is 0.5-1h.
6. the method that a kind of multi-substituent aniline according to claim 1 prepares diazonium salt, which is characterized in that the step
Pulverizer in e is flour mill, and exit is equipped with 300 meshes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810771358.2A CN109096145A (en) | 2018-07-13 | 2018-07-13 | A kind of method that multi-substituent aniline prepares diazonium salt |
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| CN201810771358.2A CN109096145A (en) | 2018-07-13 | 2018-07-13 | A kind of method that multi-substituent aniline prepares diazonium salt |
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| CN109096145A true CN109096145A (en) | 2018-12-28 |
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Citations (7)
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| CN101613304A (en) * | 2009-07-30 | 2009-12-30 | 天津德凯化工股份有限公司 | A kind of method for preparing anilines diazosalt solid powder |
| CN103435437A (en) * | 2013-09-06 | 2013-12-11 | 黑龙江省科学院石油化学研究院 | Method for synthesizing 4-(trans, trans-4-alkylcyclohexyl) fluorobenzene liquid crystal monomer compounds |
| CN103664683A (en) * | 2012-09-21 | 2014-03-26 | 浙江龙盛集团股份有限公司 | Continuous diazotization production process of aromatic amine |
| CN104610066A (en) * | 2015-02-16 | 2015-05-13 | 衢州学院 | Method for preparing 2,5-difluoro-4,6-dinitroresorcin |
| CN105330574A (en) * | 2015-09-22 | 2016-02-17 | 大连理工大学 | Waste acid treatment method after diazotization reaction of weakly alkaline arylamine |
| CN105801433A (en) * | 2016-04-12 | 2016-07-27 | 叶芳 | 4-amino-3-fluorophenol and synthesizing method thereof |
| CN106349170A (en) * | 2016-08-02 | 2017-01-25 | 东华大学 | Preparation method of 1,3-dimethyl-5-phenyluracil |
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| CN103664683A (en) * | 2012-09-21 | 2014-03-26 | 浙江龙盛集团股份有限公司 | Continuous diazotization production process of aromatic amine |
| CN103435437A (en) * | 2013-09-06 | 2013-12-11 | 黑龙江省科学院石油化学研究院 | Method for synthesizing 4-(trans, trans-4-alkylcyclohexyl) fluorobenzene liquid crystal monomer compounds |
| CN104610066A (en) * | 2015-02-16 | 2015-05-13 | 衢州学院 | Method for preparing 2,5-difluoro-4,6-dinitroresorcin |
| CN105330574A (en) * | 2015-09-22 | 2016-02-17 | 大连理工大学 | Waste acid treatment method after diazotization reaction of weakly alkaline arylamine |
| CN105801433A (en) * | 2016-04-12 | 2016-07-27 | 叶芳 | 4-amino-3-fluorophenol and synthesizing method thereof |
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Application publication date: 20181228 |