CN101914034A - Method for preparing N,N-diethyl M-Methyl Benzoyl amide - Google Patents
Method for preparing N,N-diethyl M-Methyl Benzoyl amide Download PDFInfo
- Publication number
- CN101914034A CN101914034A CN2010102653945A CN201010265394A CN101914034A CN 101914034 A CN101914034 A CN 101914034A CN 2010102653945 A CN2010102653945 A CN 2010102653945A CN 201010265394 A CN201010265394 A CN 201010265394A CN 101914034 A CN101914034 A CN 101914034A
- Authority
- CN
- China
- Prior art keywords
- diethyl
- methyl
- methyl benzoyl
- water
- stirring
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to a method for preparing N,N-diethyl M-Methyl Benzoyl amide. The method comprises the steps of: orderly adding ethidene diamine, water and benzol in a reactor, stirring and adding M-Methyl Benzoyl formyl chloride and acid absorbing fine preparation, maintaining reaction under a room temperature, stirring and reacting for 1 to 5 hours after completely adding materials, adding water to wash after finishing reaction, stirring, layering, removing water layer, distilling, removing solvent benzol so as to obtain the products of N,N-diethyl M-Methyl Benzoyl amide. In the amidation step of the method, sodium hydroxide is used as acid absorbing fine preparation so as to obtain the produces with high purity and shallow color. The product can be sold without high vacuum refining. The quality of the product totally meets the demand of technical index.
Description
Technical field
The invention belongs to the organic compound preparation field, especially a kind of N, the preparation method of N-diethyl-m-methyl benzamide.
Background technology
In industrial production, cosmetic industry are produced, N, the N-diethyl-m-methyl benzamide has more and more widely application as a kind of important organic compound and additive.N, the common production method of N-diethyl-m-methyl benzamide is direct amidate action, with organic amine as acid absorber, the problem that this type of preparation method exists: the product colour that 1, makes is darker, impurity is more, be difficult to as production marketing, must carry out further refining could the use as raw material, as the refinement treatment etc. that reduces pressure, 2, owing to need to use expensive high-vacuum pump to realize in the decompression refinement treatment step, this method production unit is many, expense is high, be difficult to reduce cost; 3, because decompression refinement treatment step is to produce N, essential and very consuming time production stage in the N-diethyl-m-methyl benzamide process, also there is the problem that the production time is long, production efficiency is low in this method.
Find that according to the retrieval patent " a kind of fixed bed one-step synthesis N; the method for N-diethyl-m-methyl benzamide " (CN101362707) discloses: stirring reaction under solvent system generates m-methyl benzoic acid diethylamine salt complex with m-methyl benzoic acid and diethylamine, get thick product to catalytic fixed bed continuously feeding constant temperature and pressure continuously dehydrating then, solvent is reclaimed in air distillation, last rectification under vacuum, get N, the pure product of N-diethyl-m-methyl benzamide, m-methyl benzoic acid: diethylamine: the solvent mol ratio is 1.0: (1.0-15.0): (0-25), mass velocity 0.1-20.0h, 60-550 ℃ of fixed bed reaction temperature, fixed bed reaction pressure 0.1-5.0MPa.
Through comparing, above-mentioned patent and the application are the difference that all there are increasing in temperature of reaction or reactions steps.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art part, the N that a kind of production unit is simple, production cost is low, production efficiency is high, product purity is high is provided, the preparation method of N-diethyl-m-methyl benzamide.
The objective of the invention is to be achieved through the following technical solutions:
A kind of N, the preparation method of N-diethyl-m-methyl benzamide is characterized in that: step is as follows:
Drop into quadrol, water, benzene successively in reactor, under agitation add m-methyl benzoyl formyl chloride and the sour finishing agent that absorbs, keep room temperature reaction, material finishes, and stirring reaction 1-5 hour, reaction was finished, and added the washing water, and stirring, standing demix are removed water layer; Solvent benzol is removed in distillation, obtains N, N-diethyl-m-methyl benzamide finished product;
It is sodium hydroxide that described acid absorbs finishing agent;
Described acid absorbs finishing agent: the weight ratio of m-methyl benzoyl formyl chloride is 0.28-0.35: 1;
Described m-methyl benzoyl formyl chloride: diethylamine: water: the weight ratio of benzene is 1: 0.5: 0.65: 1.25.
And the weight ratio of described washing water and m-methyl benzoyl formyl chloride is 0.25: 1.
And described reactor comprises refrigerating unit, whipping appts and temperature measuring equipment.
Advantage of the present invention and positively effect are:
1, this N, in the preparation method's of N-diethyl-m-methyl benzamide the amidation step, use sodium hydroxide to absorb finishing agent as acid, the product purity that obtains is higher, of light color, do not need the high vacuum refinement treatment promptly to can be used as product sells, and quality product meets the technical requirements fully.
2, this preparation method uses sodium hydroxide to absorb finishing agent as acid, and it is extensive, cheap to have raw material sources, uses also safer advantage.
3, there are not reaction process such as High Temperature High Pressure in the preparation method who the present invention relates to, has easy to operately, and the technology characteristic of simple is fit to large-scale industrial production, enhances productivity.
Embodiment
The invention will be further described below by specific embodiment, and following examples are descriptive, is not determinate, can not limit protection scope of the present invention with this.
Embodiment 1
A kind of N, the preparation method of N-diethyl-m-methyl benzamide, step is as follows:
(1) amidation reaction steps
Have that refrigerating unit, electricity stir, drop into 80 kilograms of quadrols, 104 kilograms in water, 200 kilograms of benzene successively in 500 liters of reactors of thermometer to one, under agitation, add 46 kilograms in 160 kilograms of m-methyl benzoyl formyl chlorides and acid absorption finishing agent sodium hydroxide simultaneously, keep room temperature reaction, material finishes, stirring reaction 1.5 hours, reaction is finished;
Interim: acid absorbs finishing agent: the weight ratio of m-methyl benzoyl formyl chloride is 0.28-0.35: 1;
M-methyl benzoyl formyl chloride: diethylamine: water: the weight ratio of benzene is 1: 0.5: 0.65: 1.25.
(2) water-washing step
Behind amidate action, obtain the oil reservoir mixed solution in add 40 kg water scouring waters, after stirring, standing demix is removed water layer wherein;
The weight ratio of washing water and m-methyl benzoyl formyl chloride is 0.25: 1.
(3) distillation desolventizing step
With the distillation of the mixed solution washed, remove solvent benzol, the distillatory temperature is below 85 ℃ and vacuum tightness 10-15mmHg, obtaining remaining liq is N, N-diethyl-m-methyl benzamide finished product, this N, N-diethyl-m-methyl benzamide content 98.0%, color is less than No. 5 (iodine colorimetric).
Embodiment 2
A kind of N, the preparation method of N-diethyl-m-methyl benzamide, step is as follows:
(1) amidation reaction steps
Have that refrigerating unit, electricity stir, drop into 80 kilograms of quadrols, 104 kilograms in water, 200 kilograms of benzene successively in 500 liters of reactors of thermometer to one, under agitation, add 48 kilograms in 160 kilograms of m-methyl benzoyl formyl chlorides and acid absorption finishing agent sodium hydroxide simultaneously, keep room temperature reaction, material finishes, stirring reaction 1.5 hours, reaction is finished;
(2) water-washing step
Behind amidate action, obtain the oil reservoir mixed solution in add 40 kg water scouring waters, after stirring, standing demix is removed water layer wherein;
(3) distillation desolventizing step
With the distillation of the mixed solution washed, remove solvent benzol, the distillatory temperature is below 85 ℃ and vacuum tightness 10-15mmHg, obtaining remaining liq is N, N-diethyl-m-methyl benzamide finished product, this N, N-diethyl-m-methyl benzamide content 98.0%, color is less than No. 5 (iodine colorimetric).
Embodiment 3
A kind of N, the preparation method of N-diethyl-m-methyl benzamide, step is as follows:
(1) amidation reaction steps
Have that refrigerating unit, electricity stir, drop into 80 kilograms of quadrols, 104 kilograms in water, 200 kilograms of benzene successively in 500 liters of reactors of thermometer to one, under agitation, add 50 kilograms in 160 kilograms of m-methyl benzoyl formyl chlorides and acid absorption finishing agent sodium hydroxide simultaneously, keep room temperature reaction, material finishes, stirring reaction 1.5 hours, reaction is finished;
(2) water-washing step
Behind amidate action, obtain the oil reservoir mixed solution in add 40 kg water scouring waters, after stirring, standing demix is removed water layer wherein;
(3) distillation desolventizing step
With the distillation of the mixed solution washed, remove solvent benzol, the distillatory temperature is below 85 ℃ and vacuum tightness 10-15mmHg, obtaining remaining liq is N, N-diethyl-m-methyl benzamide finished product, this N, N-diethyl-m-methyl benzamide content 98.0%, color is less than No. 5 (iodine colorimetric).
Claims (3)
1. N, the preparation method of N-diethyl-m-methyl benzamide is characterized in that: step is as follows:
Drop into quadrol, water, benzene successively in reactor, under agitation add m-methyl benzoyl formyl chloride and the sour finishing agent that absorbs, keep room temperature reaction, material finishes, and stirring reaction 1-5 hour, reaction was finished, and added the washing water, and stirring, standing demix are removed water layer; Solvent benzol is removed in distillation, obtains N, N-diethyl-m-methyl benzamide finished product;
It is sodium hydroxide that described acid absorbs finishing agent;
Described acid absorbs finishing agent: the weight ratio of m-methyl benzoyl formyl chloride is 0.28-0.35: 1;
Described m-methyl benzoyl formyl chloride: diethylamine: water: the weight ratio of benzene is 1: 0.5: 0.65: 1.25.
2. N according to claim 1, the preparation method of N-diethyl-m-methyl benzamide is characterized in that: the weight ratio of described washing water and m-methyl benzoyl formyl chloride is 0.25: 1.
3. N according to claim 1, the preparation method of N-diethyl-m-methyl benzamide is characterized in that: described reactor comprises refrigerating unit, whipping appts and temperature measuring equipment.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010102653945A CN101914034A (en) | 2010-08-28 | 2010-08-28 | Method for preparing N,N-diethyl M-Methyl Benzoyl amide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010102653945A CN101914034A (en) | 2010-08-28 | 2010-08-28 | Method for preparing N,N-diethyl M-Methyl Benzoyl amide |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101914034A true CN101914034A (en) | 2010-12-15 |
Family
ID=43321713
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2010102653945A Pending CN101914034A (en) | 2010-08-28 | 2010-08-28 | Method for preparing N,N-diethyl M-Methyl Benzoyl amide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101914034A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107840805A (en) * | 2017-10-25 | 2018-03-27 | 常州大学 | A kind of continuous synthesis N, the method for N diethyl-m-methyl benzamides |
| CN112724033A (en) * | 2020-12-16 | 2021-04-30 | 山东天安化工股份有限公司 | Synthesis method and application of deet |
| CN115073317A (en) * | 2022-07-06 | 2022-09-20 | 青岛三力本诺新材料股份有限公司 | Binuclear acid-binding agent and method for synthesizing diethyltoluamide |
-
2010
- 2010-08-28 CN CN2010102653945A patent/CN101914034A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107840805A (en) * | 2017-10-25 | 2018-03-27 | 常州大学 | A kind of continuous synthesis N, the method for N diethyl-m-methyl benzamides |
| CN112724033A (en) * | 2020-12-16 | 2021-04-30 | 山东天安化工股份有限公司 | Synthesis method and application of deet |
| CN115073317A (en) * | 2022-07-06 | 2022-09-20 | 青岛三力本诺新材料股份有限公司 | Binuclear acid-binding agent and method for synthesizing diethyltoluamide |
| CN115073317B (en) * | 2022-07-06 | 2023-01-31 | 青岛三力本诺新材料股份有限公司 | Binuclear acid-binding agent and method for synthesizing diethyltoluamide |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103319315A (en) | Method for producing aggregate-type hindered phenol antioxidant | |
| CN101914034A (en) | Method for preparing N,N-diethyl M-Methyl Benzoyl amide | |
| CN102584596A (en) | Method for preparing age inhibitor 3100 | |
| CN102875371A (en) | Method for synthesizing cyclohexyl acetate from cyclohexene | |
| CN102351694A (en) | Preparation method of trifluoroacetic acid ethyl ester | |
| CN102633635B (en) | Clean production method of dipentaerythritol hexaacrylate | |
| CN107868053B (en) | Preparation method of alkyl sulfate | |
| CN102079706A (en) | Synthesis method of hindered phenol antioxidant 1010 | |
| CN101941916A (en) | Method for refining high-purity N, N-diethyl-3-methylbenzamide | |
| CN110590532A (en) | Green synthesis method of aromatic acid | |
| CN101906035A (en) | Refining method of high-purity butyl stearate | |
| CN102863337A (en) | Synthesis method of 1,6-hexanediol diacrylate | |
| CN113480401A (en) | Synthesis method of chloro-n-pentane | |
| CN101914015B (en) | Preparation and purification method of butyl stearate | |
| CN105271306A (en) | Method for purifying cyan chloride crude product | |
| CN104003871B (en) | Butyl benzyl phthalate rectifying low-boiling-point substance is utilized to prepare the method for jasmal | |
| CN105037192B (en) | One-step method octane rating promoter is to formamido alkyl ether benzene synthetic method | |
| CN104072473A (en) | Technology for synthesizing fluoroethylene carbonate with fluosilicic acid | |
| CN104926658A (en) | Preparation technology for catalytically synthetizing L-(+)-diethyl tartrate by using strong acid cation exchange resin as catalyst | |
| CN115819188B (en) | Preparation method of 4-tert-butyl-2- (alpha-methylbenzyl) phenol | |
| CN102295574B (en) | Method for synthesizing theanine | |
| CN101941896B (en) | Method for recovering solvent acetone in production of N-(1-naphthyl) ethylenediamine dihydrochloride | |
| CN102585047A (en) | Method for preparing solvent-based peroxide di-(3, 5, 5-trimethyl hexanoyl) with mass fraction of 75 percent | |
| CN100503716C (en) | Preparation process of thermal stabilizer of tin methyl thio hydroacetate tin isooctoate for PVC | |
| CN107954859A (en) | A kind of method for separating acrylic acid/triisobutylene azeotropic mixture |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20101215 |