- Method for synthesizing N,N-dimethylaminopropyl acrylamide by utilizing decarboxylation reaction
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The invention discloses a method for synthesizing N,N-dimethylaminopropylacrylamide by utilizing a decarboxylation reaction. The method is characterized by comprising the following steps: dropwisely adding 3-dimethylaminopropylamine into a mixed solution of maleic anhydride and a solvent, stirring, reacting to obtain an intermediate, adding catalysts DMAP and DCC into the intermediate, reacting to produce Barton ester, adding a catalytic amount of tributyltin, AIBN and a polymerization inhibitor, carrying out a reaction to remove one molecule of CO2, and carrying out reduced pressure distillation to obtain a high-purity product. According to the invention, a low-temperature reaction route is used, reaction conditions are mild, and production is safer.
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- Method for catalytically preparing dimethylaminopropyl acrylamide
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The invention discloses a method for preparing dimethylaminopropylacrylamide by catalysis, and relates to the technical field of dimethylaminopropylacrylamide preparation, and the method comprises thefollowing steps: (1) adding methyl methoxypropionate and N, N-dimethyl propane diamine into a reaction kettle according to a molar ratio of 1.1-1.3, adding a catalyst and a polymerization inhibitor,and starting heating; (2) after the reaction is finished, distilling off methanol and N, N-dimethyl propane diamine generated by the reaction at 110-125 DEG C under the pressure of 15-30mmHg; (3) after distilling off the methanol and the N, N-dimethylpropane diamine to obtain an intermediate, heating the reaction kettle to 160-200 DEG C, distilling off methanol generated in the reaction process while reacting, and reacting for 6-8 hours; and (4) rectifying the reacted liquid, and collecting fractions under the pressure of 2-20 mmHg and the temperature of 90-140 DEG C so as to obtain the required dimethylaminopropylacrylamide. The method has the advantages of easily available raw materials, high yield and the like.
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Paragraph 0034; 0037; 0041-0043; 0046-0047; 0050-0051; 0054
(2020/05/30)
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- Method for synthesizing acrylamide derivative
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The invention relates to a method for synthesizing an acrylamide derivative from alkyl primary amine and acrylamide as raw materials and belongs to the field of chemical product synthesis methods. Themethod for synthesizing the acrylamide derivative comprises the following steps: 1) under conditions of 150-160 DEG C and 0.6-1MPa, conducting a Diels-Alder reaction on acrylamide and anthracene so as to obtain an acrylamide addition intermediate of 1:1; 2) conducting backflowing on the addition intermediate, alkyl primary amine and a catalyst for 6-20 hours at 50-180 DEG C, and conducting an amino exchange reaction so as to obtain an acrylamide derivative addition intermediate; and 3) carrying out thermal cracking on the acrylamide derivative addition intermediate at 150-180 DEG C and 1-3kPa, conducting rectification so as to obtain an acrylamide derivative, conducting sublimation recycling on anthracene, and repeating the process. The method for synthesizing the acrylamide derivative, which is provided by the invention, is free of liquid solvent, is capable of effectively reducing the content of VOCs (volatile organic compounds) in the generation process, and is simple in reaction process, easy in product and recycling raw material separation, easy in reaction condition control, high in security, high in reaction yield, small in byproduct amount, simple in aftertreatment, high in product purity and easy in industrial production.
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Paragraph 0029; 0042; 0046
(2019/10/01)
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- Effect of Association on Nucleophilic Addition of (Meth)acrylic Aminoamides to Acrylic Acids in Aqueous Solutions
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Reactions of nucleophilic addition of N-(3-dimethylaminoalkyl)(meth)acrylamides to acrylic, N-acryloylaminoacetic, and 2-acrylamido-2-methylpropanesulfonic acid with the formation of betaines revealed an unusual dependence of the initial rate and equilibrium conversion on concentration of the reagents. The observed effects were explained by structural features of the reagents and the products.
- Kazantsev,Baruta,Kamorin,Shirshin,Sivokhin
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p. 641 - 645
(2018/06/14)
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- Preparation method of single-functionality or multi-functionality acrylamide type compounds
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The present invention relates to the field of new material fine chemicals, particularly to a new mild, efficient and economical preparation process technology of a class of single-functionality or multi-functionality acrylamide type compounds, wherein the materials are important alkene-containing unsaturated compounds, and are increasingly used in radiation polymerization curing materials or medical application materials and other fields.
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Paragraph 0021
(2018/07/06)
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- Preparation method of acrylamide-based compounds
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The present invention relates to the field of fine chemical materials, particularly to a new mild, efficient and economical preparation process technology of a class of acrylamide-type compounds, wherein a beta-amine substituted propionamide precursor is subjected to an in-situ amine elimination reaction under the action of a suitable electrophilic reagent so as to prepare the target product.
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Paragraph 0024
(2018/01/11)
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- Method for preparing DMAPPA (N-(3-dimethyl aminopropyl) acrylamide) through catalytic amidation
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The invention belongs to the field of organic synthesis and particularly relates to a method for preparing DMAPPA (N-(3-dimethyl aminopropyl) acrylamide) through catalytic amidation. According to the method, methyl acrylate, N,N-dimethyl-1,3-propanediamine, a catalyst and an inhibitor are added to a reaction kettle, stirred, heated and cooled, excessive solvent is steamed out, an intermediate product is subjected to reduced pressure distillation treatment, then a distillate is added to a fractionating tower, reduced-pressure heating is performed for collection of a product distillate, and DMAPPA with the purity higher than or equal to 98% is obtained. The process developed with the method is simple and convenient to operate, a few reaction steps are included, and the raw material methyl acrylate is low in cost, easy to obtain and convenient to store and transport; methyl alcohol is generated in a reaction process, so that the reaction temperature is reduced, reaction conditions are mild, and side reactions are reduced; the novel catalyst is selected, accordingly, the reaction speed is high, the yield is high, the product quality is good, polymerization in a tower due to high temperature and high material activity in a distillation process is avoided, and three wastes are hardly generated.
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Paragraph 0039; 0040; 0041
(2016/10/17)
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- Preparation method of N,N-dimethyl propyl acrylamide
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The invention provides a method for utilizing solid super base as a catalyst to perform amidation reaction so as to prepare N,N-dimethyl propyl acrylamide. The method overcomes the shortcomings of multiple side reactions, low yield, much waste residues and the like produced due to the fact that sodium methoxide is used as a catalyst in the prior art, is mild in reaction, simple in operation, few in side reaction and high in yield. The reaction device requirements are not high in the reaction process, and reaction devices are not corroded. The method is environmentally friendly, is low in cost, is suitable for industrial production and has considerable advantages compared with the prior art.
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Paragraph 0004; 0020; 0021
(2016/10/10)
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- METHOD OF PRODUCING N-SUBSTITUTED (METH)ACRYLAMIDE
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PROBLEM TO BE SOLVED: To provide a method of producing N-substituted (meth)acrylamide of high purity under mild conditions. SOLUTION: This invention relates to a method of obtaining N-substituted (meth)acrylamide [3] by the detachment of an amine compound through the liquid-phase thermal decomposition of an aminopropionic acid amide derivative [1] in the presence of a catalyst mainly composed of silica, wherein R1-R5 are represented by H, a C1-32 alkyl group, and a hydroxyalkyl group. COPYRIGHT: (C)2016,JPOandINPIT
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Paragraph 0054; 0059; 0060
(2018/12/12)
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- Method For Producing Alkaline (Meth)Acrylamides
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The invention relates to a method for producing alkaline amides or imides of ethylenically unsaturated C3 to C6 carboxylic acids by reacting amines that contain at least one primary and/or secondary amino group and at least one tertiary amino group with ethylenically unsaturated C3 to C6 carboxlic acids to form an ammonium salt and said ammonium salt is subsequently converted into the alkaline amide or imide by means of microwave radiation, with the proviso that the primary and/or secondary amino group is devoid of alkoxy groups.
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Page/Page column 7
(2010/03/02)
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- METHOD FOR THE CONTINUOUS PRODUCTION OF ALKYL AMINO ACRYL AMIDES
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The invention relates to a method for the continuous production of alkyl amino acryl amides by reacting alkyl acrylates with high-boiling amines. A specific preparation technique is used in order to achieve hitherto unobtainable product qualities. Very high spatial, temporal and overall yields can also be obtained.
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Page/Page column 15-16
(2008/06/13)
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- Study of the chemoselectivity in the aminolysis reaction of methyl acrylate catalysed by lipase B from Candida antarctica
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The aminolysis reaction of methyl acrylate (MA) with N,N-dimethyl-1,3- propanediamine (DMAPA) in organic solvents has been optimised using lipase B from Candida antarctica (CAL-B) as biocatalyst. A kinetic study about the influence of the reactant concentrations, organic solvent, temperature and enzyme form has been developed focused on minimising the formation of the Michael addition products. The economic efficiency of this process has been finally investigated by reusing the enzyme in the best reaction conditions, thereby observing no significant loss of activity after three reaction cycles.
- Torre, Oliver,Gotor-Fernandez, Vicente,Alfonso, Ignacio,Garcia-Alles, Luis Fernando,Gotor, Vicente
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p. 1007 - 1014
(2007/10/03)
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- Process for the production of N-substituted acrylic acid amides
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The present invention relates to a process for the production of N-substituted acrylic acid amides by conversion of 2-carboalkoxy-t-oxabicyclo(2,2,1)hept-5-enes with primary or secondary amines to 2-carboxamide-7-oxabicyclo(2,2,1)hept-5-enes and the thermal decomposition of the latter, preferably in the presence of Lewis acids and in a vacuum, to furane and N-substituted acrylic acid amides. The process according to the invention results in high purity N-substituted acrylic acid amides that are, in the main, free of bifunctional monomers which would disrupt the subsequent polymerization of the N-substituted acrylic acid amides by undesired cross-linking.
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- Method for making N-substituted acrylamides
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The invention relates to a process for the preparation of N-substituted acrylamides of the general formula STR1 wherein Y denotes a bivalent straight - or branched chain radical with 2 to 30, preferably 2 to 18, and particularly 2 to 6 carbon atom-, preferably a group of the formula (Y1)m -(Y2)n -(Y3)t, in which Y1, Y2 and Y3 each stands for an alkylene group or the radical of a cyclic organic ring system with 5 or 6 carbon atoms, and the sum of m, n, and t is 2 or 3, and R1 denotes hydrogen or the radical of an amine of the formula N(R2) (R3), wherein R2 and R3 stand for alkyl radicals with 1 to 4 carbon atoms, which method is characterized in that dihydracrylic acid amide of the general formula STR2 is transmitted with amines of the general formula with elimination of ammonia and the resulting N-substituted β-carboxylic acid amides are converted into the desired N-substituted acrylamides at elevated temperatures by splitting out of water. The conversion of the N-substituted acrylamides with splitting out of water is preferably effected in the presence of a catalyst. The splitting out of water is preferably carried out at a temperature of 100° to 200° C. The second stage (splitting out of water) follows batch-wise at 70° to 200° C. or continuously at 250° to 450° C.
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- Process for the manufacture of α,β-unsaturated N-substituted carboxylic acid amides
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Process for the manufacture of α,β-unsaturated N-substituted carboxylic acid amides of the general formula STR1 in which R1 represents H or CH3 R2 represents H or CH3, and Y represents a divalent straight-chain or branched organic radical having 2-30 carbon atoms, and R3 represents H or the radical of an amine of the formula --N(R4)(R5), in which R4 and R5 represent alkyl radicals having 1 to 4 carbon atoms, by reacting β-substituted carboxylic acid amides of the formula STR2 in which Z represents OH or the radical R6 O--, in which R6 is an alkyl radical having 1 to 4 carbon atoms, with amines of the general formula at temperatures in the range of 100° to 200° C., preferably 120° to 175° C., with the elimination of ammonia, and heating the resulting N-substituted β-hydroxycarboxylic or β-alkoxycarboxylic acid amides in the presence of catalysts, water or alcohol, respectively, being split off. The water is split off at temperatures of 100°-250° C. with acidic catalysts such as phosphoric acid, or basic catalysts such as sodium hydroxide, and alcohol is split off at 70°-150° C. with basic catalysts such as sodium or potassium hydroxide. The reaction product is separated by distillation, optionally in vacuo.
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