- CO-production method 3 - nitro -2 - methyl benzoic acid and 3 -nitrophthalic acid (by machine translation)
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The method comprises the following steps: (3 -) in nitric acid, oxidizing -2 - nitro-3 - methylbenzoic acid to 1 nitro 3 - methylbenzoic acid under the presence of a catalyst and an initiator; and (3 -) filtering to obtain the -2 -nitro 2 methylbenzoic acid crude product after the reaction is completed by heating while carrying out the reaction to complete the reaction and completing a 3 - nitro -2 -2 - methylbenzoic acid crude product after the reaction is completed, and the obtained crude 3 - product -2 - is obtained by recrystallizing the 4 mother liquor in the mother 3 - 1 liquor step (3) after the reaction is complete and the reaction is complete and the 3 - process is completed by carrying out the reaction on the 3 - mother liquor in the presence of a 3 - catalyst and an initiator to obtain the 3 -nitrobenzoic acid crude product. The method solves the problems of large waste water waste salt amount, difficult aftertreatment and serious environmental pollution in the prior art. (by machine translation)
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Paragraph 0019-0044
(2020/07/15)
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- Method for co-production 2-methyl-6-nitrobenzoic acid and 3-nitro-2-methylbenzoic acid
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The invention discloses a method for co-production of 2-methyl-6-nitrobenzoic acid and 3-nitro-2-methylbenzoic acid. The method is characterized by comprising the following steps: (1) feeding 3-nitro-o-xylene and dilute nitric acid into an oxidation reaction kettle, carrying out heating, and conducting reacting under certain pressure by using oxygen as an oxidant; (2) after the reaction is finished, discharging an oxidation reaction solution to obtain a crude product; (3) washing the crude product with water, conducting esterifying, and performing distilling to recover a solvent after the reaction is finished, thereby obtaining an esterified concentrated solution; (4) adding alkali into the esterification concentrated solution to adjust a pH value, carrying out layering, and distilling anorganic layer under reduced pressure to recover 3-nitro-2-nitrobenzoic acid; and (5) extracting a water layer with an organic solvent, adjusting an pH value with an acid, and performing filtering anddrying to obtain the 2-methyl-6-nitrobenzoic acid. In a low-concentration nitric acid environment, 3-nitro-2-nitrobenzoic acid is produced and 2-methyl-6-nitrobenzoic acid is co-produced with oxygen used as an oxidizing agent, so the problems of low selectivity of 3-nitro-o-xylene in an oxidation process and high risks in a concentrated nitric acid oxidation process are solved.
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Paragraph 0022; 0025; 0028; 0033
(2020/10/14)
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- Naphthalenes Oxidation by Aqueous Sodium Hypochlorite Catalyzed by Ruthenium Salts under Phase-Transfer Catalytic Conditions
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Highly effective and fast oxidation of naphthalene(s) to phthalic acid(s) under biphasic conditions using nominal catalyst loading (0.5 mol%) of ruthenium chloride, 2.5 mol% tetrabutyl ammonium bromide as phase transfer catalyst and inexpensive aqueous sodium hypochlorite (NaOCl) as reagent has developed. Recovery, regeneration and reuse of the catalytic system add its merit to green chemistry.
- Patil, Rajendra D.,Sasson, Yoel
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p. 991 - 997
(2016/04/20)
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- Preparation of 2-phenyl-3-hydroxyquinoline-4(1H)-one-5-carboxamides as potential anticancer and fluorescence agents
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The synthesis of 3-hydroxyquinoline-4(1H)-one derivatives bearing substituted phenyl in position 2 and variously substituted carboxamide group in position 5 is described, with use of 3-nitrophthalic anhydride, α-haloketones and primary amines as the starting materials. The synthetic approach was inspired by the preparation of analogous derivatives reported previously. However, a different strategy had to be developed with the corresponding bis(phenacyl)-3-aminophthalates as the key intermediates. Synthesized hydroxyquinolinones, as well as their intermediates, were tested for their cytotoxic activity towards various cancer and non-malignant cell lines. The fluorescent properties of these compounds have also been evaluated. In both fields, interesting data were obtained and compared to isomeric compounds that have been studied in the past.
- Funk, Petr,Motyka, Kamil,D?ubák, Petr,Znojek, Pawel,Gurská, Soňa,Kusz, Joachim,McMaster, Claire,Hajdúch, Marián,Soural, Miroslav
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p. 48861 - 48867
(2015/06/16)
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- Inclusion complex containing epoxy resin composition for semiconductor encapsulation
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The invention is an epoxy resin composition for sealing a semiconductor, including (A) an epoxy resin and (B) a clathrate complex. The clathrate complex is one of (b1) an aromatic carboxylic acid compound, and (b2) at least one imidazole compound represented by formula (II): wherein R2 represents a hydrogen atom, C1-C10 alkyl group, phenyl group, benzyl group or cyanoethyl group, and R3 to R5 represent a hydrogen atom, nitro group, halogen atom, C1-C20 alkyl group, phenyl group, benzyl group, hydroxymethyl group or C1-C20 acyl group. The composition has improved storage stability, retains flowability when sealing, and achieves an effective curing rate applicable for sealing delicate semiconductors.
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- Design, synthesis and in-vitro cytotoxicity of novel platinum (II) complexes with phthalate as the leaving group
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Three platinum (II) complexes (6-8) with phthalate as the leaving group were synthesized and characterized by FTIR, 1H NMR, 13C NMR, mass spectrometry and elemental analysis. In-vitro cytotoxicity of all three complexes was evaluated using COLO 205 (human colon cancer cell line) against the parent drug "oxaliplatin". The compound 4-amino-(transcyclohexane-1,2-diamine) platinum(II) (8) showed potent cytotoxicity with IC50 = 0.12 μM as compared to oxaliplatin (IC50 = 0.19 μM) and its aqueous solubility was found to be 16 mg/mL which is higher than oxaliplatin (8 mg/mL). The acute toxicity showed that the platinum complex (8) was less toxic than oxaliplatin. Molecular oxaliplatin-DNA complex structure indicates that the diaminocyclohexane (DACH) and Pt (II) showed interactions with N7 and O6 of GG base pairs of DNA helix. In this present study, it is interesting to note that all three platinum based anticancer agents with phthalate as the leaving group exhibited great cytotoxicity, less toxicity, good lipophilicity as well as better aqueous solubility. 2013 Bentham Science Publishers.
- Sharma, Rajiv,Rawal, Ravindra K.,Malhotra, Manav,Gaba, Tripti,Sharma,Bhardwaj
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p. 872 - 878
(2013/12/04)
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- Rational design of colorimetric reagent for sensitivity and selectivity enhancement for β hydroxy acid of simvastatin
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Simvastatin is used in the treatment of hypercholesterolemia as β hydroxy acid of simvastatin (BHA) which inhibits 3-hydroxy methyl glutaryl coenzyme A involved in cholesterol synthesis. The present communication deals with the development of colorimetric method for estimation of BHA through rational design of colorimetric reagent for sensitivity and selectivity enhancement. BHA is an active metabolite as well as impurity of simvastatin, synthesized by alkaline hydrolysis of simvastatin. In the developed colorimetric method, improvement in the sensitivity of quantification of BHA was found to be more than 660 folds. The detector response for BHA in colorimetric method was found to be linear in concentration range of 0.1- 3.2ng/mL. This method was validated using ICH Q2B (R1) guidelines. The reported method is found to be simple, precise, accurate, rapid and economic for quantification of BHA. The colorimetric method can be optimized further for quantification of BHA in simvastatin formulations and in plasma.
- Bhatia, Manish S.,Jadhav, Swapnil D.,Dhavale, Rakesh P.,Choudhari, Prafulla B.
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p. 496 - 501
(2013/08/23)
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- Synthesis, characterization and thermal properties of some new azopolyimides
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A new class of aromatic azopolyimides were synthesized from aromatic diamine with 3,3',4,4'-azobenzenetetracarboxlic dianhydride. The synthesis involved the reaction of the dianhydride with respective diamine to yield an intermediate, soluble, open chain
- Logesh,Rajendiran
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experimental part
p. 3033 - 3038
(2012/08/29)
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- Process development for ABT-472, a benzimidazole PARP inhibitor
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A nine-step convergent process was developed for the synthesis of ABT-472, a benzimidazole PARP inhibitor. The identity and origin of several impurities were determined, and the process was modified to reduce or eliminate these impurities. A number of safety and control issues were investigated. The original synthesis was shortened to 9 steps and streamlined while maintaining a convergent strategy. A stable salt was selected, and control of the API solid form was established. The process was successfully scaled up to provide 8.5 kg of final product of >99% purity in 33% yield over 9 steps.
- Barkalow, Jufang H.,Breting, Jeffrey,Gaede, Bruce J.,Haight, Anthony R.,Henry, Rodger,Kotecki, Brian,Mei, Jianzhang,Pearl, Kurt B.,Tedrow, Jason S.,Viswanath, Shekhar K.
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p. 693 - 698
(2012/12/29)
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- HYDRAZIDES AND DERIVATIVES PRODUCTION PROCESS FROM HYDRAZINES AND DICARBOXYLIC ACIDS
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The present invention describes a process to form hydrazides from the reaction of a hydrazine and a dicarboxylic, using a Lewis acid as a main reagent of the reaction. The reaction occurs in a safe reactional environment, utilizing smooth conditions, neither involving high temperatures nor high pressures, producing the desired products with high yields, between 90-95%. The invention also describes a kit for utilization of chemiluminescent substances, comprised of two solutions.
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Page/Page column 7
(2008/06/13)
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- PIPERIDINE DERIVATIVES HAVING CCR3 ANTAGONISM
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The invention provides low molecular compounds having activity which inhibits binding of CCR3 ligands to CCR3 on target cells, i.e. CCR3 antagonists. The invention also provides compounds represented by formula (I) below, pharmaceutically acceptable acid adducts thereof, or pharmaceutically acceptable C1-C6 alkyl adducts thereof, as well as pharmaceutical compositions comprising them as effective ingredients, which are useful for treatment or prevention of diseases associated with CCR3, such as asthma and allergic rhinitis.
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- Process for introducing a carboxyl group to an aromatic carboxylic acid or a derivative thereof
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Disclosed is a process for introducing a carboxyl group to an aromatic carboxylic acid or a derivative thereof, which comprises reacting a starting aromatic carboxylic acid, such as a benzoic acid, a biphenylcarboxylic acid, a naphthalenecarboxylic acid, a diphenylcarboxylic acid, or a derivative thereof, with a carbon tetrahalide in the presence of a cyclodextrin and an alkali metal hydroxide, thereby introducing a carboxyl group to the aromatic ring of the starting aromatic carboxylic acid or the derivative thereof in substitution for a hydrogen atom bonded thereto. By the process of the present invention, a desired aromatic polycarboxylic acid or a derivative thereof can be easily obtained with high selectivity.
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- Process for separating mixtures of 3- and 4-nitrophthalic acid
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A novel improved process for separating mixtures of 3- and 4-nitrophthalic acid is described. The said process comprises treating a mixture of 3- and 4-nitrophthalic acid, which mixture is free from inorganic acid residues, in an aqueous-organic medium containing 1-20 percent by volume of water, at a temperature of between 20° and 100° C., stepwise with a base capable of forming salts of 3- and 4-nitrophthalic acid, which salts are essentially insoluble in the reaction medium, the treatment being carried out by adding base until a pH value of about 2.8 is obtained, separating the precipitating product consisting mainly of a 3-nitrophthalic acid mono-salt, subsequently precipitating, by the addition of further base, a product consisting principally of a 4-nitrophthalic acid salt, and finally converting the resulting nitrophthalic acid salts separately into the corresponding free acids, and optionally purifying these. The 3- and 4-nitrophthalic acid can be obtained by the process according to the invention in a simple manner in an isomer-free form and in good to very good yields.
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- Process for making dinitrotoluene
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Nitrated derivatives of aromatic compounds are obtained by contacting the latter, in the presence of methylene chloride as a reaction medium, with concentrated nitric acid in the presence of concentrated sulfuric acid, and thereafter isolating the formed nitro derivatives.
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