- Preparation method of sodium o-methylphenoxyacetate in synthesis process of sodium 2-methyl-4-chlorophenoxyacetate
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The invention relates to a preparation method of sodium o-methylphenoxyacetate in a synthesis process of sodium 2-methyl-4-chlorophenoxyacetate. The invention provides a preparation method of sodium o-methylphenoxyacetate, which comprises the following steps of: reacting o-cresol with sodium hydroxide to obtain a sodium o-cresol solution, reacting chloroacetic acid with sodium hydroxide to obtain a sodium chloroacetate solution, and reacting the sodium o-cresol with sodium chloroacetate under the condition of a catalyst to obtain the sodium o-methylphenoxyacetate. The catalyst is added in the preparation process, so that the reaction temperature and the decomposition rate of sodium chloroacetate can be effectively reduced, the conversion rate of o-cresol is improved, the problems of difficulty in later phenol-containing wastewater treatment and high energy consumption caused by low conversion rate of o-cresol are solved, and the preparation process is effectively simplified. Meanwhile, the sodium o-methylphenoxyacetate prepared by the preparation method is relatively high in purity and yield.
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Paragraph 0067; 0069; 0072-0090
(2021/08/14)
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- Synthetic method of 2-methyl-4-chlorophenoxyacetic acid
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The invention discloses a synthetic method of 2-methyl-4-chlorophenoxyacetic acid, and relates to the technical field of organic synthesis. The target product 2-methyl-4-chlorophenoxyacetic acid is prepared by taking o-methylphenol as a raw material, reacting with sodium chloroacetate udner the effect of sodium bicarbonate; neutralizing by hydrochloric acid to obtain a midbody 2-methyl phenoxyacetic acid; finally, chloridizing the midbody 2-methyl phenoxyacetic acid by chlorine. The method applies sodium bicarbonate to replace sodium hydroxide to carry out neutralization, the neutralization reaction is small in heat release and few in side product; the method is good for improving product content and yield; besides, the chorine is applied to chloridize, and methylbenzene is used as the solvent; the generated acid is used as the neutralizing acid of the next batch, thus the massive phenolic wastewater is reduced, and it can meet the requirement of modern green pesticide; carbon dioxideis discharged from the neutralization reaction, the reaction heat is reduced, and the energy consumption is reduced. Compared with an original technique, the reaction technique has obvious advantagesof high yield, few wastes and low energy consumption.
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Paragraph 0018; 0020; 0030; 0031
(2018/03/26)
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- Novel pyrazolone derivatives and corresponding europium(III) complexes: Synthesis and properties research
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A series of pyrazolone derivatives ligands L1?7 were successfully synthesized and validated by 1H NMR and MS, corresponding europium complexes [EuL1?7(NO3)2]NO3·EtOAc were synthesized. Physico-chemistry properties of title complexes were determined by Elemental analysis, Molar conductance, UV absorption spectra, IR spectra and Thermogravimetric analysis. The title complexes exhibit characteristic red fluorescence of Eu3+. The effect of various substituent groups in ligands on the of title Eu3+ complexes is ordered: Cl > -Br > -OCH3 > -F > -CH3 > -H > -NO2, and [EuL6(NO3)2]NO3·EtOAc containing Cl possesses the strongest fluorescence intensity, so does fluorescence quantum yield. The electrochemical properties indicate that energy gap Eg and LUMO energy level are huge affected by substituent groups, and variation trends of LUMO energy level affected by diverse substituent groups are also different. The prepared title europium complexes have potential application prospects in the fields of photoelectric functional materials and life sciences.
- Li, Dewei,Xiong, Suhao,Guo, Tiantong,Shu, Dehua,Xiao, Haihua,Li, Guizhi,Guo, Dongcai
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- Preparation method for 2,4-dichlorophenoxyacetic acid
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The invention provides a preparation method for 2,4-dichlorophenoxyacetic acid. The preparation method comprises the following steps: reacting phenol with a chloridizing agent under the action of a catalyst so as to obtain 2,4-dichlorophenol, wherein the catalyst is a composite catalyst composed of at least one metallic compound and at least one ether compound; reacting 2,4-dichlorophenol with analkaline compound so as to obtain 2,4-dichlorophenate; reacting haloacetic acid with an alkaline compound so as to obtain haloacetate; reacting the 2,4-dichlorophenate with the haloacetate so as to obtain 2,4-dichlorophenoxyacetate; and acidifying the 2,4-dichlorophenoxyacetate so as to obtain 2,4-dichlorophenoxyacetic acid. According to the invention, the specific composite catalyst is added in the chlorination process of phenol, so the prepared 2,4-dichlorophenoxyacetic acid contains few by-products, has high purity and yield, and is friendly to environment.
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Paragraph 0040; 0043; 0046; 0049; 0052; 0053; 0055; 0058
(2018/09/29)
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- Preparation method for 2,4-dichlorophenoxyacetic acid
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The invention provides a preparation method for 2,4-dichlorophenoxyacetic acid. The preparation method comprises the following steps: a) reacting 2,4-dichlorophenol with alkali to obtain a 2,4-dichlorophenolate reaction solution, drying the 2,4-dichlorophenolate reaction solution so as to obtain a 2,4-dichlorophenolate solid, reacting haloacetic acid with an alkali so as to obtain a haloacetate reaction solution and carrying out drying so as to obtain a haloacetate solid; B) reacting the 2,4-dichlorophenolate solid with the haloacetate solid so as to obtain 2,4-dichlorophenoxyacetate; and C) acidifying the 2,4-dichlorophenoxyacetate so as to obtain 2,4-dichlorophenoxyacetic acid. According to the invention, the 2,4-dichlorophenolate reaction solution and the haloacetate reaction solution are separately dried to remove water; and the 2,4-dichlorophenolate solid and the haloacetate solid are subjected to a reaction in a non-aqueous phase, so the reaction is more thorough, and the prepared 2,4-dichlorophenoxyacetic acid has high yield and purity.
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Paragraph 0053; 0054; 0056; 0058; 0060; 0062
(2018/09/29)
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- Method for preparing sodium chloroacetate
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The invention provides a method for preparing sodium chloroacetate, and belongs to the technical field of organic synthesis. The method is characterized by comprising the step that sodium silicate and chloroactic acid takes a reaction at room temperature in reaction media to produce sodium chloroacetate and silicic acid, wherein the mol ratio of the sodium silicate to the chloroactic acid is 1 to 2. The sodium silicate and the chloroactic acid are used as basic raw materials; the basic principle of preparing weak acid by strong acid is used for generating water insoluble silicic acid and sodium chloroacetate capable of being easily dissolved; through simple filtering and separation, a sodium chloroacetate water solution is obtained; filter cake silicic acid then takes a reaction with the sodium hydroxide to obtain a sodium silicate water solution.
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Paragraph 0023-0038
(2017/10/05)
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- Preparation method for cyanoacetic acid and derivatives thereof
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The invention discloses a preparation method for cyanoacetic acid and derivatives thereof. According to the invention, a mixed solution of cyanoacetic acid and sodium chloride is subjected to continuous chromatographic separation so as to obtain a cyanoacetic acid solution and sodium chloride; so the cyanoacetic acid solution with low chloride ion content or high-content solid cyanoacetic acid products and derivatives thereof are obtained, and the disadvantages of considerable decomposition and low yield of cyanoacetic acid in traditional distillation, concentration and separation are overcome. The preparation method is simple to operate, low in production cost, high in product yield and low in the amounts of waste gas, waste water and industrial residues, is an environment-friendly clean production method and can prepare the cyanoacetic acid solution with low chloride ion content or high-content solid cyanoacetic acid products and derivatives thereof.
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Paragraph 0022; 0023; 0024; 0025; 0026; 0027; 0028-0045
(2016/12/01)
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- Gel emulsifier midbody N - dodecyl betaine apparatus for producing
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The utility model provides a gel emulsifier midbody N dodecyl betaine apparatus for producing mainly includes: 12 tertiary amine storage tanks, feedstock pump, neutralizing tank are in, and pump, reation kettle, finished product pump, relation of connection between this apparatus for producing component parts does: 12 tertiary amine storage tanks are connected with feedstock pump, and feedstock pump is connected with reation kettle, and reation kettle is connected with the pump in with is connected with the neutralizing tank with the pump in, and reation kettle is connected with finished product pump, wherein, are 12 tertiary amine storage tanks horizontal tank, full volume 6.9 8.11m3, diameter of drum 1300 - 1650mm, 2650 - 4700mm of length, head thickness 8.1 - 8.9mm, is feedstock pump single -stage and single -suction centrifugal pump, rotational speed 2800 2890rmin, flow 7.9 11.5m3h, lift 32.5 34m, power 1.47 2.01KW, reation kettle nominal volume 620 does 900L press from both sides cover capacity 295 530L, the outer pot diameter 1150 1300mm, agitation speed 63 75rmin.
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Paragraph 0013; 0014; 0015; 0016
(2017/01/12)
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- Anion coordination selective [Mn3] and [Mn4] assemblies: synthesis, structural diversity, magnetic properties and catechol oxidase activity
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Syntheses, crystal structures, magnetic properties and catechol oxidation behavior are presented for [Mn3] and [Mn4] aggregates, [MnIII2MnII(O2CMe)4(dmp)2(H2O)2]·2H2O (1·2H2O), [MnIII2MnII(O2CCH2Cl)4(dmp)2(H2O)2]·H2O·MeOH (2·H2O·MeOH), [MnIII4(μ3-O)(dmp)4(μ-DMSO)(N3)(DMSO)(H2O)]ClO4·DMSO (3·ClO4·DMSO), and [MnIII4(μ3-O)(dmp)4(μ-DMSO)(ClO4)(DMSO)(H2O)]ClO4·DMSO (4·ClO4·DMSO), developed with single type ligand H2dmp, 2-[(2-hydroxy-1,1-dimethyl-ethylimino)-methyl]-phenol. The successful isolation of 1-4 resulted from a systematic exploration of the effect of MnII salts, added carboxylates, Mn/H2dmp ratio, presence of azide, and other reaction conditions. The cores of 1 and 2 are similar and consist of a linear MnIIIMnIIMnIII unit in a carboxylate and H2dmp environment, revealing a central MnII ion in a different environment and terminal MnIII ions available for the introduction of structural and magnetic anisotropy to the system. The cores of 3 and 4 are also similar and consist of a distorted incomplete-adamantane type Mn4 coordination assembly in a carboxylate-free environment built on a triangular [MnIII3(μ3-O)] unit. The magnetic behavior of complexes 1-3 is dominated by antiferromagnetic exchange coupling that results in ground state spin values of S = 3/2 for 1 and 2 and S = 0 for 3. In solution, all four complexes 1-4 show catechol oxidation activity towards 3,5-DTBC. The catalytic activity for the oxidation of 3,5-DTBC in air followed the order 4 3 1 2.
- Pait, Moumita,Shatruk, Michael,Ray, Debashis
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p. 11741 - 11754
(2015/06/30)
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- Synthesis, characterization and performance of unsaturated long-chain carboxybetaine and hydroxy sulfobetaine
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The unsaturated long-chain carboxybetaine and hydroxy sulfobetaine were synthesized by the reaction of unsaturated octadecyl tertiary amine with sodium chloroacetate and 3-chloro-2-hydroxypropanesulfonic acid sodium salt, respectively. The structures of the two betaines were characterized by IR and 1H-NMR spectroscopy. The Krafft points of the two betaines are below 0 C and the isoelectric points are at pH 8.2 and 8.0, respectively. The surface tensions (γ CMC) at the critical micelle concentrations (CMC) were measured to investigate the surface activities of the prepared compounds when the pH is equal to 4.0, 6.5 and 10.0 at 50 C, respectively. Meanwhile, the corresponding saturated betaines were synthesized and determined for comparison. The double bond in the non-polar tail leads to a slightly higher CMC and a lower γ CMC. Though the CMC of the unsaturated betaine is slightly higher than that of saturated betaine for the double bond in the non-polar tail, the applied range of the unsaturated betaine is broader than corresponding saturated betaine for low Krafft point. The CMC and ΓCMC of the four betaines increase, but the pC20 decreases, with increasing pH. As a whole, the impact of pH on the performance of the four betaines is not very obvious.
- Dong, Shuang-Jian,Li, Yun-Ling,Song, Yong-Bo,Zhi, Li-Fei
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p. 523 - 529
(2013/07/26)
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- Inhibition of monoamine oxidase by 8-phenoxymethylcaffeine derivatives
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A recent study has reported that a series of 8-benzyloxycaffeines are potent and reversible inhibitors of both human monoamine oxidase (MAO) isoforms, MAO-A and -B. In an attempt to discover additional caffeine derivatives with potent MAO inhibitory activities, and to contribute to the known structure-activity relationships of MAO inhibition by caffeine derived compounds, the present study investigates the MAO inhibitory potencies of series of 8-phenoxymethylcaffeine and 8-[(phenylsulfanyl)methyl]caffeine derivatives. The results document that the 8-phenoxymethylcaffeine derivatives act as potent reversible inhibitors of MAO-B, with IC50 values ranging from 0.148 to 5.78 μM. In contrast, the 8-[(phenylsulfanyl)methyl]caffeine derivatives were found to be weak inhibitors of MAO-B, with IC50 values ranging from 4.05 to 124 μM. Neither the 8-phenoxymethylcaffeine nor the 8-[(phenylsulfanyl)methyl]caffeine derivatives exhibited high binding affinities for MAO-A. While less potent than the 8-benzyloxycaffeines as MAO-B inhibitors, this study concludes that 8-phenoxymethylcaffeines may act as useful leads for the design of MAO-B selective inhibitors. Such compounds may find application in the therapy of neurodegenerative disorders such as Parkinson's disease. Using molecular docking experiments, this study also proposes possible binding orientations of selected caffeine derivatives in the active sites of MAO-A and -B.
- Okaecwe, Thokozile,Swanepoel, Abraham J.,Petzer, Anél,Bergh, Jacobus J.,Petzer, Jacobus P.
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experimental part
p. 4336 - 4347
(2012/08/28)
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- BENZYL-SUBSTITUTED TETRACYCLIC HETEROCYCLIC COMPOUNDS AS PDE5 INHIBITORS
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The present invention pertains to Benzyl-substituted tetracyclic heterocyclic compounds, as well as the resulting pharmaceutical compositions, and their use in the treatment or prophylaxis of diseases alleviated by inhibition of type 5 phosphodiesterases. Furthermore, the present invention pertains to the methods of manufacturing these Benzyl-substituted tetracyclic heterocyclic compounds.
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Page/Page column 107
(2010/04/03)
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- OPTICALLY ACTIVE METHOXYIMINOACETAMIDE DERIVATIVES, PROCESS FOR THE PREPARATION OF THEM, INTERMEDIATES THEREFOR, AND PESTICIDES CONTAINING THEM AS THE ACTIVE INGREDIENT
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An optically active methoxyiminoacetamide derivative represented by the following general formula (I) (in the above general formula, Ar represents an aryl group or a heteroaryl group, Y represents a hydrogen atom, a halogen atom, a C1-C4alkyl group, a C1-C4haloalkyl group, a C1-C4alkoxy group, a C1-C4haloalkoxy group, a C1-C4alkylthio group, a C2-C6alkynyloxy group, a cyano group, a nitro group or an aryl group and n is an integer of 1 to 3), wherein its angle of rotation shows a negative value in chloroform has markedly excellent activities as agricultural chemicals.
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- Ion-exchange equilibrium in synthesis of acids on KU-2(H) cation exchanger and of salts on KB-4P-2 cation exchanger
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Advisability of ion-exchange synthesis of acids on strongly acidic KU-2 cation exchanger and of salts on weakly acidic KB-4P-2 cation exchanger is studied.
- Saidakhmedov,Arslanov,Vulikh
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p. 211 - 215
(2007/10/03)
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- Chemically modified bilirubin oxidase
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A bilirubin oxidase derivative resulting from chemical modification of a water-soluble polymeric substance. The chemically modified bilirubin oxidase is useful as a drug for treating jaundice.
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- Allyl ester of 2-cyclopentyloxyacetic acid compositions
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Described are allyl ester of 2-cyclopentyloxyacetic acid, mixtures of same with 3,3-dimethyl-1-penten-4-oyl cyclohexane and/or methoxyisobutyl pyrazine and/or 3,3-dimethyl-1-(2-propenyl)-1-acetylcyclohexane, perfumery uses thereof and intermediates used in preparing said allyl ester, the allyl ester of 2-cyclopentyloxyacetic acid having the structure: STR1 the 3,3-dimethyl-1-penten-4-oyl cyclohexane having the structure: STR2 the methoxyisobutyl pyrazine having the structure: STR3 and the 3,3-dimethyl-1-(2-propenyl)-1-acetylcyclohexane having the structure: STR4
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