CN104058986B - The method of a kind of microwave radiation preparation to exalgine - Google Patents
The method of a kind of microwave radiation preparation to exalgine Download PDFInfo
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- CN104058986B CN104058986B CN201410252116.4A CN201410252116A CN104058986B CN 104058986 B CN104058986 B CN 104058986B CN 201410252116 A CN201410252116 A CN 201410252116A CN 104058986 B CN104058986 B CN 104058986B
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Abstract
The present invention relates to the method for a kind of microwave radiation preparation to exalgine, said method comprising the steps of: open-chain crown ether, acetic acid and zinc powder mix and carry out microwave radiation processing by (1), obtain mixture; (2) mixture is carried out reflow treatment under microwave radiation condition and the water of generation is steamed; (3) product that step (2) obtains is poured into be equipped with in the beaker of cold water, stir and crystallisation by cooling, obtain crystal; (4) crystal cold water cleaned and drain, obtaining thick to exalgine; (5) thick exalgine is mixed with water, heated and boiled, after oily matter dissolves completely, add gac stir and boil, mixture is filtered, by filtrate crystallisation by cooling, crystal cold water cleaned and drains, obtaining exalgine.It is short to there is the reaction times to the method for exalgine in the present invention's preparation, the advantage that products collection efficiency is high.
Description
Technical field
The invention belongs to exalgine field, relate in particular to the method for a kind of microwave radiation preparation to exalgine.
Background technology
Be colourless acicular crystal to exalgine, fusing point is 153 DEG C, and boiling point is 307 DEG C, and flash-point is 168 DEG C, and relative density is 1.212.Water is slightly soluble in exalgine, is dissolved in alcohol, ether, ethyl acetate, glacial acetic acid and hot water.Be a kind of important organic synthesis intermediate to exalgine, in chemical and medicine industry industry, there is important using value, can be obtained by acetylization reaction with open-chain crown ether.
According to bibliographical information, the acetylation reagent of open-chain crown ether has Glacial acetic acid (CH
3cOOH), acetic anhydride ((CH
3cO)
2) and Acetyl Chloride 98Min. (CH
3cOCl) etc.Wherein excess acetyl chloride is the most violent, and acetic anhydride takes second place, and Glacial acetic acid is the slowest.Glacial acetic acid low price, simple to operate, therefore normal take Glacial acetic acid as acetylation reagent.Glacial acetic acid is as acetylation reagent, and react reversible, productive rate is low, in order to reduce the generation of reversed reaction, needing the water of managing except dereaction generates, adding excessive Glacial acetic acid simultaneously, therefore have long reaction time, the shortcoming that products collection efficiency is low.
Summary of the invention
The object of the invention is to overcome the productive rate of prior art preparation to exalgine existence low, the shortcoming of long reaction time, provides a kind of method prepared exalgine, and make the productive rate of product to exalgine high, the reaction times is short.
For this reason, the invention provides the method for a kind of microwave radiation preparation to exalgine, said method comprising the steps of:
(1) by open-chain crown ether, acetic acid and zinc powder in mass ratio for 1:1.2-1.6:0.01-0.03 mixes and carry out microwave radiation processing, microwave irradiation power is 110-150w, and microwave irradiation time is 2-6min, obtains mixture;
(2) mixture carried out reflow treatment under microwave radiation condition and steamed by the water of generation, microwave irradiation power is 60-100w, and return time is 6-10min;
(3) product that step (2) obtains is poured into be equipped with in the beaker of cold water, stir and crystallisation by cooling, obtain crystal;
(4) crystal cold water cleaned and drain, obtaining thick to exalgine;
(5) thick exalgine is mixed with water, heated and boiled, after oily matter dissolves completely, add 0.5-1.5g gac stir and boil 5-10min, mixture is filtered, by filtrate crystallisation by cooling, crystal cold water cleaned and drains, obtaining exalgine.
According to the present invention, zinc powder can prevent aniline oxidized in the reaction, and zinc powder is without spark phenomenon under microwave radiation state, and reaction is rear and product is easily separated, and result of use is good.
According to the present invention, in step (1), microwave irradiation power is preferably 100-130w, and microwave irradiation time is preferably 3-6min.Microwave radiation can make open-chain crown ether and acetic acid carry out acylation reaction.
According to the present invention, in step (2), microwave irradiation power is preferably 60-80w, and return time is preferably 8-10min.
According to the present invention, in step (5), the quality optimization of gac is 1-1.5g.
According to the present invention, in step (5), boiling time is preferably 6-8min.Thick exalgine is mixed also heated and boiled can make fully to be dissolved in the water to exalgine with water, be convenient to decolouring and removing impurity.
Technical scheme of the present invention replaces traditional electric mantle heating method to heat reactant with microwave heating method, carry out microwave radiation heating is even, and microwave radiation can make key reactive force be destroyed, and can reduce the energy needed for reaction, thus reduction energy consumption of reaction, Reaction time shorten.Microwave was opened in the short period of time can reach reflux state, enters response behaviour, and the side reaction reduced to a certain extent in temperature-rise period occurs, and can improve the productive rate of product.
Embodiment
Below the specific embodiment of the present invention is described in detail.Should be understood that, embodiment described herein, only for instruction and explanation of the present invention, is not limited to the present invention.
Embodiment 1
8.56g open-chain crown ether, 12g acetic acid and 0.2g zinc powder mixed and carry out microwave radiation processing, arranging microwave irradiation power is 130w, and microwave irradiation time is 3min.The mixture obtained is carried out reflow treatment under microwave radiation condition and is steamed by the water of generation, arranging microwave irradiation power is 80w, and return time is 8min.Being poured into by the product obtained is equipped with in the beaker of cold water, stirs and crystallisation by cooling, obtains crystal; Crystal cold water cleaned and drains, obtaining thick to exalgine; Thick exalgine is mixed with water, heated and boiled, after oily matter dissolves completely, add 1g gac stir and boil 6min, mixture is filtered, by filtrate crystallisation by cooling, crystal cold water cleaned and drains, obtaining 10.5g to exalgine.
Embodiment 2
8.56g open-chain crown ether, 13.5g acetic acid and 0.25g zinc powder mixed and carry out microwave radiation processing, arranging microwave irradiation power is 120w, and microwave irradiation time is 4min.The mixture obtained is carried out reflow treatment under microwave radiation condition and is steamed by the water of generation, arranging microwave irradiation power is 90w, and return time is 9min.Being poured into by the product obtained is equipped with in the beaker of cold water, stirs and crystallisation by cooling, obtains crystal; Crystal cold water cleaned and drains, obtaining thick to exalgine; Thick exalgine is mixed with water, heated and boiled, after oily matter dissolves completely, add 1g gac stir and boil 6min, mixture is filtered, by filtrate crystallisation by cooling, crystal cold water cleaned and drains, obtaining 10.7g to exalgine.
Embodiment 3
9.18g open-chain crown ether, 12.9g acetic acid and 0.25g zinc powder mixed and carry out microwave radiation processing, arranging microwave irradiation power is 100w, and microwave irradiation time is 6min.The mixture obtained is carried out reflow treatment under microwave radiation condition and is steamed by the water of generation, arranging microwave irradiation power is 60w, and return time is 10min.Being poured into by the product obtained is equipped with in the beaker of cold water, stirs and crystallisation by cooling, obtains crystal; Crystal cold water cleaned and drains, obtaining thick to exalgine; Thick exalgine is mixed with water, heated and boiled, after oily matter dissolves completely, add 1.5g gac stir and boil 6min, mixture is filtered, by filtrate crystallisation by cooling, crystal cold water cleaned and drains, obtaining 11.3g to exalgine.
Comparative example 1
8.56g open-chain crown ether, 12g acetic acid and 0.2g zinc powder are mixed and heats with electric mantle, Heating temperature is 105 DEG C, heat-up time is 60min, the mixture obtained is carried out reflow treatment in a heated condition and the water of generation is steamed, being poured into by the product obtained is equipped with in the beaker of cold water, stir and crystallisation by cooling, obtain crystal; Crystal cold water cleaned and drains, obtaining thick to exalgine; Thick exalgine is mixed with water, heated and boiled, after oily matter dissolves completely, add 1g gac stir and boil 6min, mixture is filtered, by filtrate crystallisation by cooling, crystal cold water cleaned and drains, obtaining 9.2g to exalgine.
Table 1 type of heating is on the impact of reaction
| Numbering | Type of heating | To the quality (g) of exalgine | Reaction times (min) |
| Embodiment 1 | Carry out microwave radiation heating | 10.5 | 11 |
| Comparative example 1 | Electric mantle heats | 9.2 | 60 |
As can be seen from Table 1, compared with electric mantle type of heating, carry out microwave radiation heating can Reaction time shorten, improves the productive rate of product.
Claims (5)
1. the method for microwave radiation preparation to exalgine, is characterized in that, said method comprising the steps of:
(1) by open-chain crown ether, acetic acid and zinc powder in mass ratio for 1:1.2-1.6:0.01-0.03 mixes and carry out microwave radiation processing, microwave irradiation power is 110-150W, and microwave irradiation time is 2-6min, obtains mixture;
(2) mixture carried out reflow treatment under microwave radiation condition and steamed by the water of generation, microwave irradiation power is 60-100W, and return time is 6-10min;
(3) product that step (2) obtains is poured into be equipped with in the beaker of cold water, stir and crystallisation by cooling, obtain crystal;
(4) crystal cold water cleaned and drain, obtaining thick to exalgine;
(5) slightly will mix with water exalgine, heated and boiled, after oily matter dissolves completely, add 0.5-1.5g gac stir and boil 5-10min, mixture is filtered, by filtrate crystallisation by cooling, crystal cold water cleaned and drains, obtaining exalgine.
2. the method for microwave radiation preparation as claimed in claim 1 to exalgine, it is characterized in that, in described step (1), microwave irradiation power is 110-130W, and microwave irradiation time is 3-6min.
3. the method for microwave radiation preparation as claimed in claim 1 to exalgine, it is characterized in that, in described step (2), microwave irradiation power is 60-80W, and return time is 8-10min.
4. the method for microwave radiation preparation as claimed in claim 1 to exalgine, it is characterized in that, in described step (5), the quality of gac is 1-1.5g.
5. the method for microwave radiation preparation as claimed in claim 1 to exalgine, it is characterized in that, in described step (5), boiling time is 6-8min.
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| CN201410252116.4A CN104058986B (en) | 2014-06-09 | 2014-06-09 | The method of a kind of microwave radiation preparation to exalgine |
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Non-Patent Citations (2)
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| 对甲基乙酰苯胺的合成;曾琦斐;《应用化工》;20110630;第40卷(第6期);第1115-1116页 * |
| 微波诱导酰胺化反应研究;廖家耀 等;《西南农业大学学报（自然科学版）》;20050228;第27卷(第1期);第118-120页 * |
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