- Synthesis, characterization and behavior in water/DMSO solution of Ru(II) arene complexes with bioactive carboxylates
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The reactions of [RuCl(μ-Cl)(η6-p-cymene)]2 with sodium carboxylates, in methanol or acetonitrile solution, afforded the complexes [RuCl(κ2O-RCO2)(η6-p-cymene)] (RCO2 = valproate, 1; aspirinate, 2; diclofenate, 3), in 79–96% yields. Analogously, [RuCl(κ2O-dfCO2)(η6-benzene)], 4, was obtained in admixture with minor by-products from [RuCl(μ-Cl)(η6-benzene)]2 and sodium/silver diclofenate. The sequential reaction of [RuCl(μ-Cl)(η6-p-cymene)]2 with sodium salicylate and PPh3 gave [Ru(κ2O,O′-salCO2)(PPh3)(η6-p-cymene)], 5, in 70% yield. The hydride complex [Ru2Cl2(μ-Cl)(μ-H)(η6-p-cymene)2], 6, was produced in 36% yield from [RuCl(μ-Cl)(η6-p-cymene)]2 and sodium formate. An optimization of the experimental work-up allowed to isolate [RuCl(μ-Cl)(η6-p-cymene)]2 with an improved yield respect to the literature (98% vs. 65%). The bidentate coordination mode of the carboxylato ligands in 1–5 was unambiguously ascertained by IR and NMR spectroscopy, moreover the solid state structure of 1 was elucidated by single crystal X-ray diffraction. Complexes 1–3 experience rapid and quantitative dissociation of the carboxylato anion in DMSO/water/NaCl mixtures, mainly converting into [RuCl2(DMSO)(η6-p-cymene)], 7.
- Biancalana, Lorenzo,Pampaloni, Guido,Zacchini, Stefano,Marchetti, Fabio
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- Preparation method of sodium valproate
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The invention discloses a preparation method of sodium valproate, which comprises the following steps of by taking 2-cyano-2-propyl valerate as a raw material and a sulfuric acid aqueous solution as a catalyst, obtaining a mixture of valproic acid and valproate at 120-160 DEG C, then hydrolyzing by using an alkali solution to obtain a valproate aqueous solution, and extracting, acidifying and rectifying to obtain valproic acid. The reaction yield can reach 76%, and the purity of valproic acid can reach 99%. Compared with the traditional mechanism of oxidizing amide into carboxylic acid by nitrous acid, the method provided by the invention avoids the pollution to the atmosphere and the water body caused by the conversion of sodium nitrite into nitrous acid in an acid environment and the further conversion of nitrous acid into nitric oxide and nitrogen dioxide gas under an acid condition, and improves the operation safety of operators at the same time; and corrosion of nitric oxide and nitrogen dioxide to equipment is avoided.
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Paragraph 0044; 0050-0052; 0058-0060; 0066-0068; 0074; ...
(2021/08/06)
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- Pharmaceutical composition with high safety, and preparation method thereof
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The invention provides a pharmaceutical composition with high safety, which is characterized in that the pharmaceutical composition contains not less than 90% of sodium valproate and not more than 0.014% of 2-methylvaleric acid; and the content of the sodium valproate is preferably not less than 95% and more preferably not less than 99%. Meanwhile, the invention also provides a preparation method and application of the pharmaceutical composition. The sodium valproate pharmaceutical composition and the preparation thereof in the invention provide an effective solution for improving the safety and the stability of the medicine. Meanwhile, the preparation method of the sodium valproate pharmaceutical composition disclosed by the invention is simple in process, high in yield, high in purity and suitable for industrial mass production.
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Paragraph 0029-0040
(2021/06/22)
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- Preparation method of sodium valproate
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The invention provides a preparation method of sodium valproate, and belongs to the technical field of medicine synthesis. The method comprises the following steps: by taking ethyl valerate as a raw material, adding a methyl tert-butyl ether solution of a pyrrole metal reagent into an ether solution of ethyl valerate, then adding halopropane, carrying out an alkylation reaction, adding a weakly acidic solution in a dropwise manner to terminate the reaction after the reaction is finished, and washing with water to obtain an intermediate product; and adding a sodium hydroxide solution into the alcohol solvent of the intermediate product, carrying out a saponification reaction, and purifying to obtain sodium valproate after the saponification reaction is finished. The method is short in reaction route, high in total yield, easily available in raw materials, low in cost, high in operability and suitable for industrialization. The total molar yield of sodium valproate prepared by the methodis greater than or equal to 86.0%, and the purity of the final product is greater than or equal to 99.5%.
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Paragraph 0033; 0036-0037; 0038; 0041-0042; 0043; 0046-0047
(2020/07/14)
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- Vpa synthesis process (by machine translation)
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The invention discloses a process for synthesizing valproic acid sodium, comprises the following processes: malonic acid diethyl ester and 1- the bromine is positive propane mutual dissolution, the mixture is slowly added at certain temperature ethanol solution of sodium ethylate, heating reflux 2 hours, to recycle ethanol 110 °C, cooling to 80 °C the following, add quantitative a water-soluble sodium bromide, added after laminating a fresh keeping 15-30% aqueous sodium hydroxide solution, for 60-70 °C hydrolysis 3 hours, the gas temperature of the temperature recovery ethanol 99 °C, cooling to 80 °C the following, and in adding hydrochloric acid and dyeworks, adding crude valproic acid dissolving dipropyl malonic acid, mixed acid forming the, mixed acid for 110-160 °C decarboxylation slowly increase and produce crudely valproic acid. Valproic acid crude product after being refined after rectification, to neutralize the sodium hydroxide aqueous solution, adding toluene reflux with water, dewatering and crystallization of the valproic acid sodium, filtering, chlorofrom washing drying to obtain the finished product. The process safety and environmental protection, good quality, low cost, is suitable for industrial production. (by machine translation)
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Paragraph 0010
(2017/03/17)
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- METHOD FOR PREPARING METAL SALT OF VALPROIC ACID
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The present invention provides a simple, safe and more efficient process for preparing metal salts of valproic acid. The process includes steps of: (i) mixing valproic acid and a metal hydroxide (either dry solid or aqueous solution) in a drier to form a reaction mixture; and (ii) removing water, which is produced during the step of mixing the valproic acid and the metal hydroxide, from the reaction mixture to obtain the desired metal salts of valproic acid.
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Page/Page column 2
(2011/04/14)
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- METHODS AND COMPOSITIONS FOR TREATING MOOD DISORDER
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The invention relates to compositions and methods for treating mood spectrum disorder. The compositions relate to novel combinations and formulations of pharmaceutical compounds for treatment of mood spectrum disorders. The methods provide for use of the compounds provided herein for the treatment of mood spectrum disorders in addition to the use of mood screens for diagnosing a patient.
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Page/Page column 45
(2008/06/13)
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- Process for the preparation of substituted acetic acids and derivatives thereof
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A process for the preparation of substituted acetic acids and derivatives thereof, having the formula STR1 wherein X is --COOH, --COOY or --CN, Y is --CH3 or --C2 H5, R1 is a saturated, branched or unbranched aliphatic radical having from 1 to 6 carbon atoms, a phenyl radical, or a phenyl radical substituted by alkyl or alkoxy groups, and R2 is hydrogen or a saturated, branched or unbranched aliphatic radical having from 1 to 6 carbon atoms, a phenyl radical, or a phenyl radical substituted by alkyl or alkoxy groups, wherein R1 and R2 may be the same or different which process comprises converting the corresponding malonic or cyanoacetic ester of the formula STR2 wherein Z is --COOY or --CN, and Y, R1 and R2 are identified as above at elevated temperature in the presence of a catalyst, e.g., a catalyst containing from about 50 to 75 weight percent SiO2 and from 15 to 19 weight percent Al2 O3 and exhibit ignition losses ranging from 15 to 20 weight percent.
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