- Synthesis method of 3-methoxyl-N, N-dimethylacrylamide
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The invention relates to a synthesis method of 3-methoxyl-N, N-dimethylacrylamide, and belongs to the technical field of chemical synthesis. The synthesis method comprises the following steps of adding 3-methoxypropionic acid and dimethylamine into a sealed reactor; raising the temperature to 80 to 150 DEG C; performing reaction to obtain 3-methoxyl-N, N-dimethylacrylamide, wherein the pressure in the sealed reactor is 0.1 to 10.0MPa. The 3-methoxypropionic acid is used as the raw materials to perform high-temperature dewatering with dimethylamine in a sealed reaction vessel; polyhydric alcohol and basic catalysts are not needed; the reaction is simple; the implementation is easy; the yield of a product is high; the purity is high; the high yield is realized; meanwhile, the pollution is little; the cost is low; the method conforms to the requirements of modern chemical green synthesis. Meanwhile, the 3-methoxypropionic acid uses low-price acrylonitrile as the starting raw materials; the acrylonitrile is subjected to alkoxylation to obtain methoxyl propionitrile; then, hydrolysis is performed. The operation is simple; the energy consumption is low.
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Paragraph 0041-0044
(2017/07/22)
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- 3-methoxy-N,N-dimethylacrylamide synthesis method
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The invention belongs to the technical field of chemical synthesis and relates to a 3-methoxy-N,N-dimethylacrylamide synthesis method. The method includes steps: adding acrylonitrile, absolute methanol and metal alkoxide into a reactor for reaction, recovering unreacted absolute methanol to obtain 3-methoxypropionitrile; adding acid catalysts and water into 3-methoxypropionitrile, heating for hydrolysis reaction, and filtering to obtain 3-methoxypropionic acid; adding 3-methoxypropionic acid and dimethylamine into a closed reactor, heating for reaction to obtain 3-methoxy-N,N-dimethylacrylamide. By adoption of cheap acrylonitrile as a starting material, the acrylonitrile is subjected to alkoxylation to obtain methoxypropionitrile which is then hydrolyzed to obtain methoxypropionic acid, and acid-base reaction, salification and dehydration are performed to obtain a target product without consumption of polyhydric alcohols and alkaline catalysts. High-temperature dehydration can be realized in the closed reactor, simplicity and feasibility in reaction are achieved, and high product yield and high purity are realized.
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Paragraph 0039; 0041; 0042
(2017/08/29)
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- Formation of a New, Strongly Basic Nitrogen Anion by Metal Oxide Modification
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Development of new hybrid materials having unique and unprecedented catalytic properties is a challenge for chemists, and heterogeneous-homogeneous hybrid catalysts have attracted much attention because of the preferable and exceptional properties that are highly expected to result from combination of the components. Base catalysts are widely used in organic synthesis as key materials, and a new class of base catalysts has made a large impact from academic and industrial viewpoints. Here, a principle for creating a new strong base by hybridization of homogeneous and heterogeneous components is presented. It is based on the modification of organic compounds with metal oxides by using the acid-base property of metal oxides. Based on kinetic and DFT studies, combination of CeO2 and 2-cyanopyridine drastically enhanced the basicity of 2-cyanopyridine by a factor of about 109 (~9 by pKa (in CH3CN)), and the pKa was estimated to be ~21, which locates it in the superbase category. 2-Cyanopyridine and CeO2 formed a unique adsorption complex via two interaction modes: (i) coordinative interaction between the Ce atom of CeO2 and the N atom of the pyridine ring in 2-cyanopyridine, and (ii) covalent interaction between the surface O atom of CeO2 and the C atom of the CN group in 2-cyanopyridine by addition of the lattice oxygen of CeO2 to the CN group of 2-cyanopyridine. These interactions established a new, strongly basic site of N- over the CeO2 surface.
- Tamura, Masazumi,Kishi, Ryota,Nakayama, Akira,Nakagawa, Yoshinao,Hasegawa, Jun-Ya,Tomishige, Keiichi
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supporting information
p. 11857 - 11867
(2017/09/08)
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- MANUFACTURING METHOD OF β-SUBSTITUTED PROPIONIC ACID AMIDE AND N-SUBSTITUTED (METH)ACRYLAMIDE
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PROBLEM TO BE SOLVED: To provide a method for industrially manufacturing β-alkoxy propionic acid amide, β-amino propionic acid amide and N-substituted (meth)acryl amide using (meth)acrylic acid ester as starting material at high yield and high purity. SOLUTION: There is provided a method for obtaining N-substituted (meth)acryl amide represented by target compound formula (7) by conducting an amidation reaction with amine using β-substituted propionic acid ester represented by the formula (1) of a product of a Michael addition reaction of (meth)acrylic acid ester and alcohol or amine in presence of a metal complex as a catalyst to obtain β-substituted propionic acid amide represented by the formula (3) and conducting a thermal decomposition reaction of β-substituted propionic acid amide in presence of the metal complex as the catalyst to eliminate alcohol or amine. A-CH2-C(R1)H-C(=O)-OR2 (1), A-CH2-C(R1)H-C(=O)-N(R3)R4 (3), CH2=C(R1)-C(=O)-N(R3)R4 (7) SELECTED DRAWING: None COPYRIGHT: (C)2018,JPOandINPIT
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Paragraph 0047; 0050; 0062
(2018/07/03)
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- METHOD FOR PRODUCING BETA -ALKOXYPROPIONAMIDE
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A method for producing a β-alkoxypropionamide including reacting a β-alkoxypropionic acid ester represented by the following formula (1) and an amine represented by the following formula (2) in the presence of a polyol and a basic catalyst, thereby to produce a β-alkoxypropionamide represented by the following formula (3), wherein, as the polyol, a reaction residue that is generated by the reaction and contains a used polyol is used: (wherein in the formulas, R and R' are independently a C1 to C6 linear, branched or cyclic, saturated hydrocarbon group; R1 and R2 are independently a C1 to C6 linear, branched or cyclic, saturated hydrocarbon group; and R3 is H or CH3).
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Paragraph 0060; 0061; 0062; 0063; 0064
(2015/03/03)
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- METHOD FOR PRODUCING ALPHA, BETA-UNSATURATED CARBOXYLIC ACID-N,N-DISUBSTITUTED AMIDE AND METHOD FOR PRODUCING 3-ALKOXYCARBOXYLIC ACID-N,N-DISUBSTITUTED AMIDE
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The invention is directed to a technique for effectively producing an amide compound suitable for use as a solvent or a detergent on a large scale and at low cost.
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- METHOD FOR PRODUCING BETA-ALKOXYPROPIONAMIDE
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A method for producing a β-alkoxypropionamide including: subjecting a β-alkoxypropionic acid ester represented by the following formula (I) and a polyol having two or more OH groups to a transesterification reaction in the presence of a basic catalyst, thereby to synthesize a transesterified polyol of a β-alkoxypropionic acid ester; andsubjecting the transesterified polyol and an amine represented by the following formula (II) to an amidation reaction, thereby to synthesize a β-alkoxypropionamide represented by the following formula (III):
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Page/Page column 3-4
(2011/10/19)
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- PROCESS FOR PRODUCING -ALKOXYPROPIONAMIDE
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A method for producing a β-alkoxypropionamide shown by the following formula (I) including the step of reacting a β-alkoxypropionic acid ester with an amine in the presence of a basic catalyst or in the presence of a basic catalyst and a polyol: wherein R1 is an alkyl group having 1 to 8 carbon atoms, and R2 and R3 are independently hydrogen, a methyl group, an ethyl group, a methoxy group, an ethoxy group, a methoxymethyl group or a glycidyl group.
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Page/Page column 8-9
(2009/12/07)
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