CN106966923B - A kind of synthetic method of 3- methoxyl group-N, N- dimethylpropionamide - Google Patents
A kind of synthetic method of 3- methoxyl group-N, N- dimethylpropionamide Download PDFInfo
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Abstract
The present invention relates to a kind of 3- methoxyl group-N, the synthetic method of N- dimethylpropionamide, belongs to technical field of chemical synthesis, includes the following steps: for acrylonitrile, anhydrous methanol and metal alkoxide to be added in reactor and react, the unreacted anhydrous methanol of recycling, obtains 3- methoxypropionitrile；Acidic catalyst and water are added into 3- methoxypropionitrile, heats hydrolysis, is filtered to obtain 3- methoxypropionic acid；3- methoxypropionic acid and dimethylamine are added in closed reactor, temperature reaction obtains 3- methoxyl group-N, N- dimethylpropionamide.The present invention is using inexpensive acrylonitrile as starting material, acrylonitrile alkoxide obtains methoxypropionitrile, it hydrolyzes to obtain methoxypropionic acid again, then acid-base reaction obtains target product at dehydration of salt and does not need polyalcohol, basic catalyst, it is dehydrated in closed reactor high temperature, easy reaction, and product yield high, purity is high.
Description
Technical field
The present invention relates to a kind of synthetic method of chemical materials intermediate more particularly to a kind of 3- methoxyl group-N, N- diformazans
The synthetic method of base propionamide, belongs to technical field of chemical synthesis.
Background technique
3- methoxyl group-N, N- dimethylpropionamide (structural formula is as shown in formula I), are a kind of colorless and transparent solvents, there is amide
Group and alkyl group can be mixed with multi-solvents, being capable of high level dissolution polymer polyamide；With highly dissoluble, height
The features such as permeability, high fluidity, low viscosity, low surface tension, and there is no irritation to skin, safety and environmental protection can be very
Conventional solvent N-Methyl pyrrolidone is substituted well, is widely used in electronics, medicine, pesticide, pigment, cleaning agent, insulation material
In the industries such as material.Nowadays in the safety solvent market that competition constantly refines, in addition to dissolubility, high volatile and low toxicity also become
The important chip of solvent competition, therefore, the wide market of product.
Synthesis for 3- methoxyl group-N, N- dimethylpropionamide, existing method is mainly with 3- methoxypropionic acid first
Ester and dimethylamine are raw material, and diethylene glycol (DEG) is that solvent synthesizes under the catalysis of sodium alkoxide.However in this method solvent diethylene glycol (DEG) because
245 DEG C of boiling point too high, recovery cost is larger, can not reuse.And catalyst sodium alkoxide dosage is larger, needs to neutralize with sulfuric acid,
Processing is refiltered, technological operation is cumbersome, generates a large amount of solid slags, does not meet environmentally protective requirement.Furthermore reaction yield
It is not high with selectivity, and dimethylamine raw material needs are significantly excessive, and production process generates the exhaust gas of a large amount of dimethylamine, to two
Methylamine gas recovery system equipment requirement is very high, invests very big.
Reaction equation is as follows:
As Chinese patent (application number: 201380019269.8) discloses a kind of manufacturer of beta-alkoxypropionamide
Method is reacted in the patent with amine using β-alkoxy acrylic ester class and manufactures beta-alkoxypropionamide, but this method with
β-alkoxy acrylic ester class is raw material, reacts with amine, needs to recycle by-product after reaction, and in the by-product recycled
Containing a large amount of amine, processing is more difficult, and raw material itself is through obtained by acroleic acid esterification, methoxylation, process is relatively complicated.
Summary of the invention
It is an object of the invention to be directed to the deficiencies in the prior art, a kind of inexpensive, high yield 3- first is provided
The synthetic method of oxygroup-N, N- dimethylpropionamide.
Above-mentioned purpose of the invention is achieved through the following technical solutions: a kind of 3- methoxyl group-N, N- dimethylpropionamide
Synthetic method, the synthetic method include the following steps:
The synthesis of S1,3- methoxypropionitrile: acrylonitrile, anhydrous methanol and metal alkoxide are added in reactor
Reaction, the unreacted anhydrous methanol of recycling obtain 3- methoxypropionitrile；
The synthesis of S2,3- methoxypropionic acid: acidic catalyst and water, heating is added in the 3- methoxypropionitrile into step S1
Reaction is hydrolyzed, is filtered to obtain 3- methoxypropionic acid；
The synthesis of S3,3- methoxyl group-N, N- dimethylpropionamide: 3- methoxypropionic acid and dimethylamine are added to closed anti-
It answers in device, temperature reaction obtains 3- methoxyl group-N, N- dimethylpropionamide.
Reaction in the prior art is essentially ester and reacts with amine, and the source of ester is to obtain acrylic acid by acroleic acid esterification
Ester, then alkoxylate obtain β-alkoxy acrylic ester, reamination.The acrylonitrile that the present invention uses price less expensive is former for starting
Material, acrylonitrile alkoxide obtains methoxypropionitrile, then hydrolyzes to obtain methoxypropionic acid, and then acid-base reaction obtains target at dehydration of salt
Product.It is because the generation of side reaction, product itself not can be used as solvent, do not need again that polyalcohol is not needed in the present invention
Dilution is the then high temperature dehydration again because reaction belongs to acid-base neutralization reaction without basic catalyst, it is easy to it carries out, if
Basic catalyst is introduced, not but not works, methoxypropionic acid can be consumed instead, while introducing impurity.Furthermore the present invention is
It avoids the volatilization of raw material amine under hot conditions and reversible reaction occurs, need to be reacted in closed space.The present invention is realizing
Pollution is reduced while high yield, meets the requirement of modern chemical industry green syt.
In the synthetic method of above-mentioned 3- methoxyl group-N, N- dimethylpropionamide, metal alkoxide described in step S1
Object is one of sodium methoxide, sodium ethoxide, potassium methoxide, potassium ethoxide, magnesium methoxide, magnesium ethylate, sodium tert-butoxide, potassium tert-butoxide or a variety of.This
Invention makees catalyst using the strong metal alkoxide of catalytic capability, and the convenient sources of metal alkoxide, be easy to get, cost is relatively low.
Preferably, metal alkoxide described in step S1 is one or both of sodium methoxide, sodium ethoxide.With it
He compares metal alkoxide, and the activity of sodium methoxide and sodium ethoxide is stronger, and cost is relatively low, has better competitiveness.
In the synthetic method of above-mentioned 3- methoxyl group-N, N- dimethylpropionamide, acrylonitrile in step S1, anhydrous methanol,
The amount of substance ratio of metal alkoxide is 1:(1-50): (0.001-0.05).The amount of substance is excessive, methanol when will lead to post-processing
Yield it is larger, in turn result in that loss is larger, and the too small concentration that will lead to substrate in reaction system is larger, to cause secondary anti-
It should increase, and then yield is caused to reduce.
Preferably, the amount of substance ratio of acrylonitrile, anhydrous methanol, metal alkoxide is 1:(5-10): (0.005-0.02).
In the synthetic method of above-mentioned 3- methoxyl group-N, N- dimethylpropionamide, the temperature of reaction described in step S1 is
20-100℃。
Preferably, the temperature of reaction described in step S1 is 50-60 DEG C.
In the synthetic method of above-mentioned 3- methoxyl group-N, N- dimethylpropionamide, the temperature of hydrolysis is in step S2
80-120℃。
Preferably, the temperature of hydrolysis is 90-100 DEG C in step S2.
In the synthetic method of above-mentioned 3- methoxyl group-N, N- dimethylpropionamide, 3- methoxypropionitrile and acid in step S2
Property catalyst amount of substance ratio be 1:1-15.
Preferably, the amount of substance of 3- methoxypropionitrile and acidic catalyst ratio is 1:1-3.
In the synthetic method of above-mentioned 3- methoxyl group-N, N- dimethylpropionamide, acidic catalyst described in step S2
For one of the concentrated sulfuric acid, hydrochloric acid, nitric acid, phosphoric acid or a variety of.
Preferably, the acidic catalyst is one or both of the concentrated sulfuric acid, hydrochloric acid.
In the synthetic method of above-mentioned 3- methoxyl group-N, N- dimethylpropionamide, the reaction temperature in step S3 is 80-
150℃.If reaction temperature is too low in step S3 of the invention, can not be dehydrated after acid-base reaction；It, can if reaction temperature is excessively high
Increase back reaction, leads to hypertonia, and then influence yield and purity.
Preferably, the reaction temperature in step S3 is 90-110 DEG C.
In the synthetic method of above-mentioned 3- methoxyl group-N, N- dimethylpropionamide, the pressure of reactor is in step S3
0.1-10.0MPa.The present invention is to avoid the volatilization of raw material amine under hot conditions with high-pressure sealed reaction and reversible reaction occurs, high
There is no exhaust gas generation under pressure confined reaction, needs to control the pressure in reactor.Equipment used in the present invention is high-pressure sealed
Equipment, such as autoclave, pressurize one of tower reactor, pressure pipeline reactor or a variety of, preferably autoclave.Pressure is excessive
It is higher to equipment requirement, become larger so as to cause investment, pressure is too small, and causing reaction, not exclusively yield is low.
Preferably, the pressure of reactor is 0.5-2Mpa in step S3.
In the synthetic method of above-mentioned 3- methoxyl group-N, N- dimethylpropionamide, 3- methoxypropionic acid and two in step S3
The amount of substance ratio of methylamine is 1:1-8.
Preferably, 3- methoxypropionic acid and the amount of substance of dimethylamine ratio are 1:1-2 in step S3.
Reaction equation of the invention is as follows:
In conclusion the present invention, using inexpensive acrylonitrile as starting material, acrylonitrile alkoxide obtains methoxypropionitrile, then water
Solution obtains methoxypropionic acid, and then acid-base reaction obtains target product at dehydration of salt and do not need polyalcohol, basic catalyst, close
The dehydration of reactor high temperature, easy reaction, and product yield high, purity is high are closed, it is dirty while realizing high yield
It contaminates less, is at low cost, meeting the requirement of modern chemical industry green syt.
Specific embodiment
The following is specific embodiments of the present invention, and technical scheme of the present invention will be further described, but the present invention is simultaneously
It is not limited to these embodiments.
3- methoxy is synthesized by the parameter in table 1 embodiment 1-38 and comparative example 3-20 and using the following method of the present invention
Base-N, N- dimethylpropionamide:
The synthesis of S1,3- methoxypropionitrile: acrylonitrile, anhydrous methanol and metal alkoxide are added in reactor
It first reacts, unreacted anhydrous methanol is recycled in redistillation, obtains 3- methoxypropionitrile；
The synthesis of S2,3- methoxypropionic acid: acidic catalyst and water is added in the 3- methoxypropionitrile into step S1, carries out
Hydrolysis is filtered to obtain 3- methoxypropionic acid；
The synthesis of S3,3- methoxyl group-N, N- dimethylpropionamide: 3- methoxypropionic acid and dimethylamine are added to closed anti-
It answers in device, temperature reaction obtains 3- methoxyl group-N, N- dimethylpropionamide.
Table 1:
It can be obtained from table 1 embodiment 1-8 and comparative example 8-11, the synthesis of 3- methoxyl group-N, N- dimethylpropionamide of the present invention
Temperature in method in the step S3 yield at 80-150 DEG C is higher, and preferably 90-110 DEG C, most preferably preferably 100 DEG C, if temperature is low
The yield of final products can be all significantly affected in 80 DEG C or higher than 150 DEG C.It can be obtained from table 1 embodiment 9-14 and comparative example 3-7,
Pressure in the synthetic method of 3- methoxyl group-N, N- dimethylpropionamide of the present invention in step S3 closed reactor is in 0.1-
Yield is higher within the scope of 10.0MPa, preferably 0.5-2Mpa, best preferred 1.5MPa.From table 1 embodiment 15-18 and comparative example 12-
14 can obtain, and the reaction temperature in the synthetic method of 3- methoxyl group-N, N- dimethylpropionamide of the present invention in step S2 is in 80-120
Yield is higher at DEG C, and preferably 90-100 DEG C, most preferably preferably 95 DEG C.It can be obtained from table 1 embodiment 19-24 and comparative example 15-17, this hair
Reaction temperature in the synthetic method of bright 3- methoxyl group-N, N- dimethylpropionamide in step S1 at 20-100 DEG C yield compared with
Height, preferably 50-60 DEG C, most preferably preferably 55 DEG C.It can be obtained from 1 embodiment 25-29 of table and comparative example 18,3- methoxyl group-N of the present invention,
In the synthetic method of N- dimethylpropionamide in step S1 the amount of substance ratio of acrylonitrile, anhydrous methanol, metal alkoxide 1:
(1-50): product yield is higher in (0.001-0.05) range.It can be obtained from 1 embodiment 30-34 of table and comparative example 19,3- of the present invention
The amount of substance of 3- methoxypropionitrile and acidic catalyst ratio in step S2 in the synthetic method of methoxyl group-N, N- dimethylpropionamide
In 1:(1-15) product yield is higher in range.It can be obtained from 1 embodiment 35-38 of table and comparative example 20,3- methoxyl group-N of the present invention,
In the synthetic method of N- dimethylpropionamide in step S3 3- methoxypropionic acid and the amount of substance of dimethylamine ratio in 1:(1-8) range
Interior product yield is higher.
In conclusion the present invention, using inexpensive acrylonitrile as starting material, acrylonitrile alkoxide obtains methoxypropionitrile, then water
Solution obtains methoxypropionic acid, and then acid-base reaction obtains target product at dehydration of salt and do not need polyalcohol, basic catalyst, close
Close the dehydration of reactor high temperature, easy reaction, and product yield high, up to 92% or more.
It randomly selects and gas phase is passed through using 3- methoxyl group-N, N- the dimethylpropionamide sample that the method for the present invention synthesizes
Chromatography is detected.The results are shown in Table 2 for the gas chromatographic analysis of sample after detection.
Table 2: result is analyzed using 3- methoxyl group-N, N- the dimethylpropionamide sample chromatogram that the method for the present invention synthesizes
| Peak number | Retention time | Peak area (uV*s) | Peak height (uV) | Purity (%) |
| 1 | 13.363 | 59.276 | 1390.806 | 0.0388 |
| 2 | 16.427 | 359842.781 | 3579131.250 | 99.9612 |
| It amounts to | 359902.057 | 3580522.056 | 100.0000 |
As can be seen from Table 2: 3- methoxyl group-N, N- the dimethylpropionamide purity synthesized using the method for the present invention compared with
Height reaches 99.9612%.
Metal alkoxide can be sodium methoxide, sodium ethoxide, potassium methoxide, potassium ethoxide, magnesium methoxide, ethyl alcohol in the above-described embodiments
One of magnesium, sodium tert-butoxide, potassium tert-butoxide are a variety of.Acidic catalyst can be one in the concentrated sulfuric acid, hydrochloric acid, nitric acid, phosphoric acid
Kind is a variety of.Wherein, amount=quality/molecular weight of substance, if metal alkoxide is sodium methoxide, propylene in citing embodiment
Nitrile, anhydrous methanol, sodium methoxide amount of substance ratio be (m acrylonitrile g/53g/mol): (m methanol g/32g/mol): (m sodium methoxide g/
54g/mol), it is also calculated with this conversion mode in other embodiments.
Specific embodiment described herein is only an example for the spirit of the invention.The neck of technology belonging to the present invention
The technical staff in domain can do various modifications or supplement or is substituted in a similar manner to described specific embodiment, but simultaneously
Spirit or beyond the scope defined by the appended claims of the invention is not deviated by.
It is skilled to this field although present invention has been described in detail and some specific embodiments have been cited
For technical staff, as long as it is obvious for can making various changes or correct without departing from the spirit and scope of the present invention.
Claims (7)
1. a kind of synthetic method of 3- methoxyl group-N, N- dimethylpropionamide, which is characterized in that the synthetic method includes such as
Lower step:
The synthesis of S1,3- methoxypropionitrile: acrylonitrile, anhydrous methanol and metal alkoxide are added in reactor instead
It answers, the unreacted anhydrous methanol of recycling obtains 3- methoxypropionitrile；
The synthesis of S2,3- methoxypropionic acid: acidic catalyst and water is added in the 3- methoxypropionitrile into step S1, and heating carries out
Hydrolysis is filtered to obtain 3- methoxypropionic acid；
The synthesis of S3,3- methoxyl group-N, N- dimethylpropionamide: 3- methoxypropionic acid and dimethylamine are added to closed reactor
In, temperature reaction obtains 3- methoxyl group-N, N- dimethylpropionamide；Wherein 3- methoxypropionic acid and the amount of substance of dimethylamine ratio are 1:
1-2；The pressure of reactor is 0.5-2MPa；Reaction temperature is 90-110 DEG C.
2. the synthetic method of 3- methoxyl group-N, N- dimethylpropionamide according to claim 1, which is characterized in that step
Metal alkoxide described in S1 is sodium methoxide, sodium ethoxide, potassium methoxide, potassium ethoxide, magnesium methoxide, magnesium ethylate, sodium tert-butoxide, uncle
One of butanol potassium is a variety of.
3. the synthetic method of 3- methoxyl group-N, N- dimethylpropionamide according to claim 1, which is characterized in that step
Acrylonitrile in S1, anhydrous methanol, metal alkoxide amount of substance ratio be 1:(1-50): (0.001-0.05).
4. the synthetic method of 3- methoxyl group-N, N- dimethylpropionamide according to claim 1, which is characterized in that step
The temperature of reaction described in S1 is 20-100 DEG C.
5. the synthetic method of 3- methoxyl group-N, N- dimethylpropionamide according to claim 1, which is characterized in that step
The temperature of hydrolysis is 80-120 DEG C in S2.
6. the synthetic method of 3- methoxyl group-N, N- dimethylpropionamide according to claim 1, which is characterized in that step
The amount of substance of 3- methoxypropionitrile and acidic catalyst ratio is 1:1-15 in S2.
7. the synthetic method of 3- methoxyl group-N, N- dimethylpropionamide according to claim 1 or 6, which is characterized in that step
Acidic catalyst described in rapid S2 is one of the concentrated sulfuric acid, hydrochloric acid, nitric acid, phosphoric acid or a variety of.
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| CN108767235B (en) * | 2018-06-04 | 2020-05-29 | 广州天赐高新材料股份有限公司 | Lithium secondary battery anode slurry and preparation method and application thereof |
| CN113105354B (en) * | 2021-03-05 | 2023-07-21 | 河南省化工研究所有限责任公司 | Method for preparing N- (4-hydroxy-3-methoxybenzyl) nonanamide without catalyst |
| CN113563228A (en) * | 2021-07-26 | 2021-10-29 | 山东汉鸿新材料科技有限公司 | Method for preparing 3-methoxypropionitrile |
| CN115043749B (en) * | 2022-06-08 | 2023-06-27 | 东华大学 | Preparation method of diamide diol |
| CN117964512B (en) * | 2024-04-01 | 2024-06-04 | 山东惟普控股有限公司 | Synthesis method of N, N-dimethyl-3-methoxy propionamide |
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