CN106966923A - A kind of synthetic method of 3 methoxyl group N, N dimethylpropionamides - Google Patents
A kind of synthetic method of 3 methoxyl group N, N dimethylpropionamides Download PDFInfo
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- CN106966923A CN106966923A CN201710160457.2A CN201710160457A CN106966923A CN 106966923 A CN106966923 A CN 106966923A CN 201710160457 A CN201710160457 A CN 201710160457A CN 106966923 A CN106966923 A CN 106966923A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C253/00—Preparation of carboxylic acid nitriles
- C07C253/30—Preparation of carboxylic acid nitriles by reactions not involving the formation of cyano groups
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C231/00—Preparation of carboxylic acid amides
- C07C231/02—Preparation of carboxylic acid amides from carboxylic acids or from esters, anhydrides, or halides thereof by reaction with ammonia or amines
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/08—Preparation of carboxylic acids or their salts, halides or anhydrides from nitriles
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts
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Abstract
The present invention relates to a kind of synthetic method of 3 methoxyl group N, N dimethylpropionamide, belong to technical field of chemical synthesis, comprise the following steps：Acrylonitrile, absolute methanol and metal alkoxide are added in reactor and reacted, the unreacted absolute methanol of recycling obtains 3 methoxypropionitriles；Acidic catalyst and water are added into 3 methoxypropionitriles, hydrolysis is heated, through filtering to obtain 3 methoxypropionic acids；3 methoxypropionic acids and dimethylamine are added in closed reactor, temperature reaction obtains 3 methoxyl group N, N dimethylpropionamides.The present invention is using inexpensive acrylonitrile as initiation material, acrylonitrile alkoxide obtains methoxypropionitrile, hydrolyze again and obtain methoxypropionic acid, then acid-base reaction obtains target product into dehydration of salt and does not need polyalcohol, base catalyst, in the dehydration of closed reactor high temperature, easy reaction, and product yield high, purity are 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 groups-N, N- diformazan
The synthetic method of base propionamide, belongs to technical field of chemical synthesis.
Background technology
3- methoxyl groups-N, N- dimethylpropionamide (structural formula is as shown in formula I), are a kind of water white transparency solvents, there is acid amides
Group and alkyl group, can be mixed with multi-solvents, being capable of high level dissolving polymer polyamide；With highly dissoluble, height
The features such as permeability, high fluidity, low viscosity, low surface tension, and there is no excitant to skin, safety and environmental protection can be very
Conventional solvent 1-METHYLPYRROLIDONE is substituted well, is widely used in electronics, medicine, agricultural chemicals, pigment, cleaning agent, insulation material
In the industries such as material.Nowadays the security solvent market constantly refined in competition, in addition to dissolubility, high volatile and low toxicity also turn into
The important chip of solvent competition, therefore, the wide market of product.
For the synthesis of 3- methoxyl groups-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 is synthesized under the catalysis of sodium alkoxide.But in this method solvent diethylene glycol (DEG) because
Boiling point is 245 DEG C too high, and recovery cost is larger, it is impossible to reuse.And catalyst sodium alkoxide large usage quantity with sulfuric acid, it is necessary to neutralized,
Processing is refiltered, technological operation is cumbersome, produce a large amount of solid slags, do not meet the requirement of environmental protection.Furthermore, reaction yield
It is not high with selectivity, and dimethylamine raw material needs significantly excessive, the waste gas of a large amount of dimethylamine of production process generation, to two
Methylamine gas recovery system equipment requirement is very high, invests very big.
Reaction equation is as follows：
Such as Chinese patent (application number：201380019269.8) disclose a kind of manufacturer of beta-alkoxypropionamide
Using β-alkoxy acrylic ester class and amine reaction manufacture beta-alkoxypropionamide in method, the patent, but this method with
β-alkoxy acrylic ester class is raw material, is reacted with amine, needs to reclaim accessory substance after reaction, and in the accessory substance reclaimed
Containing substantial amounts of amine, processing is more difficult, and raw material is through obtained by acroleic acid esterification, methoxylation, process is relatively complicated in itself.
The content of the invention
It is an object of the invention to for the deficiencies in the prior art, there is provided a kind of low cost, 3- first in high yield
The synthetic method of epoxide-N, N- dimethylpropionamide.
The above-mentioned purpose of the present invention is achieved through the following technical solutions：A kind of 3- methoxyl groups-N, N- dimethylpropionamide
Synthetic method, described synthetic method comprises the following steps：
The synthesis of S1,3- methoxypropionitrile：Acrylonitrile, absolute methanol and metal alkoxide are added in reactor
Reaction, the unreacted absolute methanol of recycling obtains 3- methoxypropionitriles；
The synthesis of S2,3- methoxypropionic acid：3- methoxypropionitriles into step S1 add acidic catalyst and water, heating
Reaction is hydrolyzed, through filtering to obtain 3- methoxypropionic acids；
The synthesis of S3,3- methoxyl group-N, N- dimethylpropionamide：3- methoxypropionic acids and dimethylamine are added to closed anti-
Answer in device, temperature reaction obtains 3- methoxyl groups-N, N- dimethylpropionamide.
Reaction of the prior art is essentially ester and reacted 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 present invention uses the less expensive acrylonitrile of price former for starting
Material, acrylonitrile alkoxide obtains methoxypropionitrile, then hydrolyzes and obtain methoxypropionic acid, and then acid-base reaction obtains target into dehydration of salt
Product.It is that, because the generation without side reaction, product can be used as solvent in itself, it is not necessary to 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 base catalyst, it is easy to carry out, if
Base catalyst is introduced, not but not is worked, methoxypropionic acid can be consumed on the contrary, while introducing impurity.Furthermore, the present invention is
Avoid the volatilization of raw material amine under hot conditions and occur reversible reaction, need to be reacted in closed space.The present invention is being realized
Pollution is reduced while in high yield, meets the requirement of modern chemical industry green syt.
In the synthetic method of above-mentioned 3- methoxyl groups-N, N- dimethylpropionamide, the metal alkoxide described in step S1
Thing is one kind or many in sodium methoxide, caustic alcohol, potassium methoxide, potassium ethoxide, magnesium methoxide, magnesium ethylate, sodium tert-butoxide, potassium tert-butoxide
Kind.The present 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, the metal alkoxide described in step S1 is one or both of sodium methoxide, caustic alcohol.With it
He compares metal alkoxide, and the activity of sodium methoxide and caustic alcohol is stronger, and cost is relatively low, with more preferable competitiveness.
In the synthetic method of above-mentioned 3- methoxyl groups-N, N- dimethylpropionamide, acrylonitrile in step S1, absolute methanol,
The amount of substance ratio of metal alkoxide is 1:(1-50):(0.001-0.05).The amount of material is excessive, methanol when can cause to post-process
Yield it is larger, in turn result in that loss is larger, the too small concentration that can cause substrate in reaction system is larger, so as to cause secondary anti-
It should increase, and then cause yield to reduce.
Preferably, the amount of substance ratio of acrylonitrile, absolute methanol, metal alkoxide is 1:(5-10):(0.005-
0.02)。
In the synthetic method of above-mentioned 3- methoxyl groups-N, N- dimethylpropionamide, the temperature reacted described in step S1 is
20-100℃。
Preferably, the temperature reacted described in step S1 is 50-60 DEG C.
In the synthetic method of above-mentioned 3- methoxyl groups-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 groups-N, N- dimethylpropionamide, 3- methoxypropionitriles and acid in step S2
Property catalyst amount of substance ratio be 1:1-15.
Preferably, the amount of substance ratio of 3- methoxypropionitriles and acidic catalyst is 1:1-3.
In the synthetic method of above-mentioned 3- methoxyl groups-N, N- dimethylpropionamide, the acidic catalyst described in step S2
For the one or more in the concentrated sulfuric acid, hydrochloric acid, nitric acid, phosphoric acid.
Preferably, described acidic catalyst is one or both of the concentrated sulfuric acid, hydrochloric acid.
In the synthetic method of above-mentioned 3- methoxyl groups-N, N- dimethylpropionamide, the reaction temperature in step S3 is 80-
150℃.If reaction temperature is too low in the step S3 of the present invention, it can not be dehydrated after acid-base reaction；, can if reaction temperature is too high
Increase back reaction, cause 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 groups-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 occur reversible reaction, high
There is no waste gas to produce, it is necessary to control the pressure in reactor under pressure confined reaction.Equipment used is high-pressure sealed in the present invention
One or more in equipment, such as autoclave, pressurization tower reactor, pressure pipeline reactor, preferably autoclave.Pressure is excessive
Higher to equipment requirement, so as to cause investment to become big, pressure is too small, causes reaction incomplete, yield is low.
Preferably, the pressure of reactor is 0.5-2Mpa in step S3.
In the synthetic method of above-mentioned 3- methoxyl groups-N, N- dimethylpropionamide, 3- methoxypropionic acids and two in step S3
The amount of substance ratio of methylamine is 1:1-8.
Preferably, 3- methoxypropionic acids and the amount of substance of dimethylamine ratio are 1 in step S3:1-2.
The reaction equation of the present invention is as follows：
In summary, the present invention is using inexpensive acrylonitrile as initiation material, and acrylonitrile alkoxide obtains methoxypropionitrile, then water
Solution obtains methoxypropionic acid, and then acid-base reaction obtains target product into dehydration of salt and do not need polyalcohol, base catalyst, close
The dehydration of reactor high temperature, easy reaction are closed, and product yield high, purity are high, it is dirty while realizing in high yield
Dye less, cost it is low, meet the requirement of modern chemical industry green syt.
Embodiment
The following is the specific embodiment of the present invention, technical scheme is further described, but the present invention is simultaneously
It is not limited to these embodiments.
By the parameter in the embodiment 1-38 of table 1 and comparative example 3-20 and using the following method synthesis 3- methoxies of the present invention
Base-N, N- dimethylpropionamide：
The synthesis of S1,3- methoxypropionitrile：Acrylonitrile, absolute methanol and metal alkoxide are added in reactor
First react, unreacted absolute methanol is reclaimed in redistillation, obtains 3- methoxypropionitriles；
The synthesis of S2,3- methoxypropionic acid：3- methoxypropionitriles into step S1 add acidic catalyst and water, carry out
Hydrolysis, through filtering to obtain 3- methoxypropionic acids；
The synthesis of S3,3- methoxyl group-N, N- dimethylpropionamide：3- methoxypropionic acids and dimethylamine are added to closed anti-
Answer in device, temperature reaction obtains 3- methoxyl groups-N, N- dimethylpropionamide.
Table 1：
It can be obtained from the embodiment 1-8 of table 1 and comparative example 8-11, the synthesis of 3- methoxyl groups-N, N- dimethylpropionamide of the present invention
Temperature in method in the step S3 yield at 80-150 DEG C is higher, 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 the embodiment 9-14 of table 1 and comparative example 3-7,
Pressure in the synthetic method of 3- methoxyl groups-N, N- dimethylpropionamide of the present invention in step S3 closed reactors is in 0.1-
Yield is higher in the range of 10.0MPa, preferably 0.5-2Mpa, optimal preferably 1.5MPa.From the embodiment 15-18 of table 1 and comparative example 12-
14 can obtain, and the reaction temperature in the synthetic method of 3- methoxyl groups-N, N- dimethylpropionamide of the present invention in step S2 is in 80-120
Yield is higher at DEG C, preferably 90-100 DEG C, most preferably preferably 95 DEG C.It can be obtained from the embodiment 19-24 of table 1 and comparative example 15-17, this hair
Reaction temperature in the synthetic method of bright 3- methoxyl groups-N, N- dimethylpropionamide in step S1 at 20-100 DEG C yield compared with
Height, preferably 50-60 DEG C, preferably most preferably 55 DEG C.It can be obtained from the embodiment 25-29 of table 1 and comparative example 18,3- methoxyl groups-N of the present invention,
In the synthetic method of N- dimethylpropionamides in step S1 the amount of substance ratio of acrylonitrile, absolute methanol, metal alkoxide 1:
(1-50):Product yield is higher in the range of (0.001-0.05).It can be obtained from the embodiment 30-34 of table 1 and comparative example 19,3- of the present invention
In the synthetic method of methoxyl group-N, N- dimethylpropionamide in step S2 3- methoxypropionitriles and acidic catalyst amount of substance ratio
1:Product yield is higher in the range of (1-15).It can be obtained from the embodiment 35-38 of table 1 and comparative example 20,3- methoxyl groups-N of the present invention,
In the synthetic method of N- dimethylpropionamides in step S3 3- methoxypropionic acids and the amount of substance of dimethylamine ratio 1:(1-8) scope
Interior product yield is higher.
In summary, the present invention is using inexpensive acrylonitrile as initiation material, and acrylonitrile alkoxide obtains methoxypropionitrile, then water
Solution obtains methoxypropionic acid, and then acid-base reaction obtains target product into dehydration of salt and do not need polyalcohol, base catalyst, close
Close the dehydration of reactor high temperature, easy reaction, and product yield high, up to more than 92%.
Randomly select 3- methoxyl groups-N, N- the dimethylpropionamide sample obtained using the inventive method synthesis and pass through gas phase
Chromatogram is detected.The gas chromatographic analysis result of sample is as shown in table 2 after detection.
Table 2：Obtained 3- methoxyl groups-N, N- dimethylpropionamide sample chromatogram analysis result is synthesized using the inventive method
| 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 |
| Amount to | 359902.057 | 3580522.056 | 100.0000 |
As can be seen from Table 2：Using the inventive method synthesize obtained 3- methoxyl groups-N, N- dimethylpropionamide purity compared with
Height, reaches 99.9612%.
Metal alkoxide can be sodium methoxide, caustic alcohol, potassium methoxide, potassium ethoxide, magnesium methoxide, ethanol in the above-described embodiments
One or more in magnesium, sodium tert-butoxide, potassium tert-butoxide.Acidic catalyst can be one in the concentrated sulfuric acid, hydrochloric acid, nitric acid, phosphoric acid
Plant or a variety of.Wherein, amount=quality/molecular weight of material, if metal alkoxide is sodium methoxide, propylene in citing embodiment
Nitrile, absolute methanol, the amount of substance ratio of sodium methoxide are (m acrylonitrile g/53g/mol)：(m methanol g/32g/mol)：(m sodium methoxides g/
54g/mol), also calculated in other embodiment with this conversion mode.
Specific embodiment described herein is only to spirit explanation for example of the invention.Technology neck belonging to of the invention
The technical staff in domain can be made various modifications or supplement to described specific embodiment or be substituted using similar mode, but simultaneously
Do not deviate by the spirit of the present invention or surmount scope defined in appended claims.
It is skilled to this area although having been made a detailed description to the present invention and being cited some specific embodiments
For technical staff, as long as it is obvious that can make various changes or correct without departing from the spirit and scope of the present invention.
Claims (10)
1. a kind of synthetic method of 3- methoxyl groups-N, N- dimethylpropionamide, it is characterised in that described synthetic method is included such as
Lower step：
The synthesis of S1,3- methoxypropionitrile：Acrylonitrile, absolute methanol and metal alkoxide are added in reactor instead
Should, the unreacted absolute methanol of recycling obtains 3- methoxypropionitriles；
The synthesis of S2,3- methoxypropionic acid：3- methoxypropionitriles into step S1 add acidic catalyst and water, and heating is carried out
Hydrolysis, through filtering to obtain 3- methoxypropionic acids；
The synthesis of S3,3- methoxyl group-N, N- dimethylpropionamide：3- methoxypropionic acids and dimethylamine are added to closed reactor
In, temperature reaction obtains 3- methoxyl groups-N, N- dimethylpropionamide.
2. the synthetic method of 3- methoxyl groups-N, N- dimethylpropionamide according to claim 1, it is characterised in that step
Metal alkoxide described in S1 is sodium methoxide, caustic alcohol, potassium methoxide, potassium ethoxide, magnesium methoxide, magnesium ethylate, sodium tert-butoxide, uncle
One or more in butanol potassium.
3. the synthetic method of 3- methoxyl groups-N, N- dimethylpropionamide according to claim 1, it is characterised in that step
Acrylonitrile, absolute methanol, the amount of substance ratio of metal alkoxide are 1 in S1:(1-50):(0.001-0.05).
4. the synthetic method of 3- methoxyl groups-N, N- dimethylpropionamide according to claim 1, it is characterised in that step
The temperature reacted described in S1 is 20-100 DEG C.
5. the synthetic method of 3- methoxyl groups-N, N- dimethylpropionamide according to claim 1, it is characterised in that step
The temperature of hydrolysis is 80-120 DEG C in S2.
6. the synthetic method of 3- methoxyl groups-N, N- dimethylpropionamide according to claim 1, it is characterised in that step
The amount of substance ratio of 3- methoxypropionitriles and acidic catalyst is 1 in S2:1-15.
7. the synthetic method of 3- methoxyl groups-N, the N- dimethylpropionamide according to claim 1 or 7, it is characterised in that step
Acidic catalyst described in rapid S2 is the one or more in the concentrated sulfuric acid, hydrochloric acid, nitric acid, phosphoric acid.
8. the synthetic method of 3- methoxyl groups-N, N- dimethylpropionamide according to claim 1, it is characterised in that step
Reaction temperature in S3 is 80-150 DEG C.
9. the synthetic method of 3- methoxyl groups-N, N- dimethylpropionamide according to claim 1, it is characterised in that step
The pressure of reactor is 0.1-10.0MPa in S3.
10. the synthetic method of 3- methoxyl groups-N, N- dimethylpropionamide according to claim 1, it is characterised in that step
3- methoxypropionic acids and the amount of substance of dimethylamine ratio are 1 in S3:1-8.
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| WO2019232837A1 (en) * | 2018-06-04 | 2019-12-12 | 广州天赐高新材料股份有限公司 | Slurry for positive electrode of secondary lithium battery, preparation method for same, and application thereof |
| CN113105354A (en) * | 2021-03-05 | 2021-07-13 | 河南省化工研究所有限责任公司 | Novel method for preparing N- (4-hydroxy-3-methoxybenzyl) nonanamine without catalyst |
| 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 |
| CN115043749A (en) * | 2022-06-08 | 2022-09-13 | 东华大学 | Preparation method of diamide diol |
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