41663-84-7Relevant articles and documents
Preparation method of N - alkyl -4 -nitrophthalimide
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Paragraph 0040; 0042; 0052; 0054-0055; 0057, (2021/10/27)
The invention discloses a preparation method of N - alkyl -4 -nitrophthalimide, which comprises the following steps of 1) mixing phthalic anhydride, alkyl aldehyde and inorganic amine, reacting under the action of hydrogen, cooling and crystallizing, and drying to obtain N -alkyl phthalimide. Step 2) The 1 alkylphthalimide obtained in step N -) is subjected to nitration reaction, and the product is purified and dried to obtain the N -alkyl -4 -nitrophthalimide. The alkyl aldehyde in step 1) is preferably an alkyl aldehyde of carbon 1 - 4. The preparation method has the advantages of wide raw material source, low price, simple process, easiness in large-scale production and the like. Through one-step synthesis, the reaction efficiency is high, the device is simple and easy to operate, and green and environment-friendly.
Olive-shaped N-methyl-4-nitrophthalimide crystal and preparation method thereof
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Paragraph 0025-0047, (2020/07/15)
The invention relates to an olive-shaped N-methyl-4-nitrophthalimide crystal and a preparation method thereof. The method comprises the steps: a) carrying out a reaction on N-methylphthalimide and fuming nitric acid in a concentrated sulfuric acid system to prepare a concentrated sulfuric acid solution of N-methyl-4-nitrophthalimide; b) pouring the concentrated sulfuric acid solution of N-methyl-4-nitrophthalimide into low-temperature water, stirring, separating out an N-methyl-4-nitrophthalimide solid, washing with water, and drying; and c) refluxing and cooling the dried N-methyl-4-nitrophthalimide solid, and then filtering and drying to obtain the olive-shaped N-methyl-4-nitrophthalimide crystal. According to the invention, the problem that heat accumulation is easy to cause danger in the production process in the prior art is solved while the problems of small product crystal stacking density, difficult feeding in downstream synthesis application and low product yield are also solved.
A process for preparing N - alkyl -4 - nitro phthalimide method (by machine translation)
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Paragraph 0046; 0047; 0048; 0055; 0056; 0057; 0061-0063, (2019/02/19)
The invention belongs to the field of organic synthesis technology, and relates to a N - alkyl phthalimide as raw materials, nitric acid as nitrating agent, through the continuous flow at low temperature the nitration reaction preparation N - alkyl - 4 - nitro phthalic acid imide series products. The reaction time is short, the production cycle is short, intermittent reaction kettle solves the problem caused by the accumulation of the raw materials, the reaction process is more stable, significantly improves the reaction efficiency. The different structure of the micro-channel in the reactor to enhance the mass transfer, heat transfer performance, keep the reaction temperature constant, to avoid the phenomenon of the rack frame, to reduce by-product, at the same time improves the safety of the reaction process. The micro-channel of the mass transfer effect of strong in the reactor, so that the liquid - liquid reaction liquid to be fully mixed, in the reaction process, concentrated sulfuric acid, can greatly reduce the consumption of nitric acid, reduces the production of waste. (by machine translation)
N-methyl-4-nitrophthalimide preparation method
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Paragraph 0071; 0075-0077; 0081-0083; 0087-0089; 0093-0095, (2019/11/20)
The invention relates to the technical field of organic synthesis processes, particularly to a N-methyl-4-nitrophthalimide preparation method, which comprises: preparation of a nitrating agent: mixinga nitrate and concentrated sulfuric acid to form a nitrating agent; preparation of N-methylphthalimide: adding methylamine and phthalic anhydride to a solvent, and carrying out heating reflux to obtain N-methylphthalimide; and preparation of N-methyl-4-nitrophthalimide: adding the nitrating agent to the N-methylphthalimide, and carrying out a reaction to form N-methyl-4-nitrophthalimide. According to the present invention, the nitrating agent is prepared at a low temperature by using nitrate and concentrated sulfuric acid so as to avoid the harm of fuming nitric acid to environmental and human body; and after the nitrating reaction is performed with the nitrating agent, the remaining nitrating agent can be recycled by extraction, and can further be added with an auxiliary agent to obtainnitrate or sulfate precipitate as a by-product, wherein ammonium nitrate or ammonium sulfate, and the like can be used as fertilizers so as to achieve environmentally friendly circulation reactions.
METHODS FOR THE MANUFACTURE OF AN AROMATIC BISIMIDE AND A POLYETHERIMIDE
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Paragraph 0072, (2017/07/14)
A method for producing an aromatic bisimide includes reacting a dialkali metal salt of a dihydroxy aromatic compound with an N-alkyl nitrophthalimide to form a product mixture including the aromatic bisimide. The N-alkyl nitrophthalimide includes 4-nitro-N-(C1-13 alkyl)phthalimide, 3-nitro-N-(C1-13 alkyl)phthalimide, or a combination including at least one of the foregoing, and 4-hydroxy-3,5-dinitro-N-(C1-13 alkyl)phthalimide in an amount of 1-10000 ppm. The aromatic bisimide can be obtained in a yield of greater than 75%, or 90-99.8%. A method for the manufacture of a polyetherimide, a polyetherimide, and an article including the polyetherimide are also disclosed. A mixed acid nitration process for the preparation of an N-alkyl nitrophthalimide is also described.
Photochemical generation of superbases from carboxylates consisting of phthalimidoacetic acid derivatives and superbases
Arimitsu, Koji,Fukuda, Ken,Sakai, Nobuhiko
, p. 831 - 833 (2014/06/23)
We have developed simple and powerful photobase generators capable of highly efficient production of superbases. These photobase generators were prepared by simply mixing phthalimidoacetic acid derivatives with the corresponding superbases. The use of photobase generators enabled anionic UV curing at lower temperatures, in contrast to previous anionic UV curing materials that required heat treatment above 150 °C after UV irradiation. The cured films showed no volume shrinkage.
A new series of N2-substituted-5-(p-toluenesulfonylamino)phthalimide analogues as α-glucosidase inhibitors
Bian, Xiaoli,Wang, Qian,Ke, Changhu,Zhao, Guilan,Li, Yiping
, p. 2022 - 2026 (2013/04/24)
Several members of a new family of non-sugar-type α-glycosidase inhibitors, bearing a 5-(p-toluenesulfonylamino)phthalimide moiety and various substituent at the N2 position, were synthesized and their activities were investigated. The newly synthesized compounds displayed different inhibition profile towards yeast α-glycosidase and rat intestinal α-glycosidase. Almost all the compounds had strong inhibitory activities against yeast α-glycosidase. Regarding rat intestinal α-glycosidase, only analogs with N2-aromatic substituents displayed varying degrees of inhibitory activities on rat intestinal maltase and lactase and nearly all compounds showed no inhibition against rat intestinal α-amylase. Structure-activity relationship studies indicated that 5-(p- toluenesulfonylamino)phthalimide moiety is a favorable scaffold to exert the α-glucosidase inhibitory activity and substituents at the N2 position have considerable influence on the efficacy of the inhibition activities.
Molecular docking and enzymatic evaluation to identify selective inhibitors of aspartate semialdehyde dehydrogenase
Luniwal, Amarjit,Wang, Lin,Pavlovsky, Alexander,Erhardt, Paul W.,Viola, Ronald E.
experimental part, p. 2950 - 2956 (2012/06/29)
Microbes that have gained resistance against antibiotics pose a major emerging threat to human health. New targets must be identified that will guide the development of new classes of antibiotics. The selective inhibition of key microbial enzymes that are responsible for the biosynthesis of essential metabolites can be an effective way to counter this growing threat. Aspartate semialdehyde dehydrogenases (ASADHs) produce an early branch point metabolite in a microbial biosynthetic pathway for essential amino acids and for quorum sensing molecules. In this study, molecular modeling and docking studies were performed to achieve two key objectives that are important for the identification of new selective inhibitors of ASADH. First, virtual screening of a small library of compounds was used to identify new core structures that could serve as potential inhibitors of the ASADHs. Compounds have been identified from diverse chemical classes that are predicted to bind to ASADH with high affinity. Next, molecular docking studies were used to prioritize analogs within each class for synthesis and testing against representative bacterial forms of ASADH from Streptococcus pneumoniae and Vibrio cholerae. These studies have led to new micromolar inhibitors of ASADH, demonstrating the utility of this molecular modeling and docking approach for the identification of new classes of potential enzyme inhibitors.
N-methylation of NH-containing heterocycles with dimethyl carbonate catalyzed by TMEDA
Zhao, Sheng-Yin,Zhang, Hai-Quan,Zhang, Deng-Qing,Shao, Zhi-Yu
experimental part, p. 128 - 135 (2011/11/01)
A practical method for N-methylation of NH-containing heterocycles using an environmentally safe and less toxic methylating reagent, dimethyl carbonate, has been developed. N,N,N',N'-tetramethylethylenediamine (TMEDA), an extremely active organocatalyst for the methylation of imides, indoles, benzimidazoles, and piperazines in conjunction with dimethyl carbonate, can lead to N-methylation products with high conversion. The reaction sequence consists of competing alkylation and acylation pathways and involves TMEDA as a nucleophilic catalyst. A possible reaction mechanism is discussed based on the reaction results.
