- 2, 3, 5, 6 - Tetrachloro - 1, 4 - benzenedicarboxylic acid dimethyl manufacturing method
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2, 3, 5, 6 - Tetrachloro - 1, 4 - benzenedicarboxylic acid dimethyl [to] horticultural herbicide useful in manufacturing, compared with conventional methods such as reducing environmentally harmful byproducts of hexachlorobenzene penta- chlorobenzene or content, can be efficiently manufactured in an industrial method. (I) formula [a]The manufacturing method of the compound represented, 2, 3, 5, 6 - tetrachloro - 1, 4 - benzenedicarboxylic acid (a), a ketone-based solvent in the presence of a hydrous alkali carbonate, prepared by reacting dimethyl sulfate, formula (I) compounds represented by the process to obtain the crystal, and (b) the crystal was washed with warm water of 30 a-°C 100, then further washed with an organic solvent comprising 30 a-°C 80, said method. [Drawing] no
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- ALKALI METAL FLUORIDE DISPERSION AND PROCESS FOR PRODUCING FLUORINE-CONTAINING ORGANIC COMPOUND USING THE SAME
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An alkali metal fluoride dispersion essentially consisting of an alkali metal fluoride and an aprotic organic solvent obtainable by conducting the following Step (A), subsequently conducting the following Step (B) at least once, and then conducting the following Step(C); Step (A): a step of separating a liquid phase from an alkali metal fluoride dispersion comprising at least one alcohol solvent selected from the group consisting of methanol, ethanol and isopropanol and an alkali metal fluoride, and mixing the separated liquid phase with an aprotic organic solvent having a boiling point of 85° C. or higher at normal pressure to obtain a mixture containing the alkali metal fluoride; Step (B): a step of obtaining a mixture containing the alkali metal fluoride comprising the following Steps (b1) to (b3); Step (b1): a step of concentrating the mixture containing the alkali metal fluoride obtained in Step (A) or Step (b3) to obtain a concentrated fraction and a concentrated residue; Step (b2): a step of mixing a residue of the alkali metal fluoride dispersion obtained by separating the liquid phase in Step (A) or a residue of the mixture obtained by separating a liquid phase in Step (b3) with the concentrated fraction obtained in Step (b1) to obtain a mixture containing an alkali metal fluoride; and Step (b3): a step of separating a liquid phase from the mixture containing an alkali metal fluoride obtained in Step (b2) and mixing the separated liquid phase with the concentrated residue obtained in Step (b1) to obtain a mixture containing an alkali metal fluoride; and Step (C): a step of removing the alcohol solvent from the mixture containing the alkali metal fluoride, which is obtained in Step (B), to obtain the alkali metal fluoride dispersion essentially consisting of the alkali metal fluoride and the aprotic organic solvent.
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Page/Page column 9
(2011/05/16)
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- POTASSIUM FLUORIDE DISPERSION SOLUTION, AND PROCESS FOR PRODUCTION OF FLUORINATED ORGANIC COMPOUND USING THE SAME
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A potassium fluoride dispersion essentially consisting of potassium fluoride and an aprotic organic solvent having a boiling point higher than that of methanol, which is obtainable by mixing a mixture containing potassium fluoride and 5 to 50 parts by weight of methanol per 1 part by weight of potassium fluoride with the aprotic organic solvent followed by concentrating the obtained mixture, and a process for producing a fluorine-containing organic compound comprising contacting an organic compound having at least one group capable of being substituted nucleophilically with a fluorine atom with the potassium fluoride dispersion.
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Page/Page column 7
(2009/04/25)
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- METHOD FOR PRODUCING TETRAFLUOROTEREPHTHALIC ACID DIFLUORIDE
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A method for producing tetrafluoroterephthalic acid difluoride comprising reacting tetrachloroterephthalic acid dichloride with potassium fluoride in the presence of dimethyl sulfone.
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Page/Page column 7
(2008/12/08)
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- Study of the Kinetics and Mechanism of the Base-Catalyzed Esterification of Tetrachloroterephthaloyl Chloride with HPLC and Carbon-13 FT-NMR
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The pyridine base-catalyzed esterification of tetrachloroterephthaloyl dichloride (R) with methanol was studied at room temperature and found to follow a four-step course; high-perfomance liquid chromatography (HPLC) was used to analyze and characterize intermediates in reaction mixtures.The reaction proceeds with the initial formation of a benzoylpyridinium ion (M) followed by formation of a terephthaloyl dipyridinium ion (N); both are strongly associated with the alcohol solvent molecules as indicated by chromatographic retention times.The pyridinium salts react with alcohol to form a monoester followed by product diester (P) at slower rates.The rate constants for each mechanistic step were obtained from batch reactor studies together with HPLC analysis; the rates for the first two consecutive steps were dependent on the organic base (pyridine and 4-picoline) catalyst concentration.Large, negative values of the entropy of activation were interpreted in terms of a highly ordered transition state in the course of formation of the ionic intermediates.The presence of alcohol was found to be important for the formation of the salts.Carbon-13 FT-NMR spectra of polychlorinated reaction intermediates were obtained at low temperature to enhance sensitivity; results supported conclusions regarding structures and reaction requirements.
- Langer, Stanley H.,Chu, Alexander H. T.,Bolme, Mark W.,Turner, Michael S.,Quinting, Gregory R.
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p. 3601 - 3648
(2007/10/02)
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- 5,6-Dihydro-1,2,4,6-thiatriazin-5-one-1,1-dioxides
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5,6-Dihydro-1,2,4,6-thiatriazin-5-one-1,1-dioxides of the formula STR1 where R1 is hydrogen, a metal atom or an unsubstituted or substituted ammonium radical, R2 is a saturated or unsaturated straight-chain aliphatic radical of up to 10 carbon atoms, a cycloaliphatic radical or 3 to 7 carbon atoms, a branched saturated or unsaturated aliphatic radical of 3 to 10 carbon atoms, a halogen-, alkoxy- or alkylmercapto-substituted aliphatic radical of 2 to 10 carbon atoms tetrahydrofuryl substituted methyl, a cycloalkoxy-substituted aliphatic radical of 4 to 10 carbon atoms, unsubstituted or halogen-substituted benzyl or phenyl, halophenyl, or alkylphenyl of a total of up to 10 carbon atoms, R3 is hydrogen, a straight-chain aliphatic radical of up to 10 carbon atoms, a cycloaliphatic radical of 3 to 7 carbon atoms, a branched aliphatic radical of 3 to 10 carbon atoms, haloalkyl, or alkoxyalkyl of 2 to 10 carbon atoms and X is oxygen and may also be sulfur if R2 is unsubstituted or halogen-substituted benzyl, processes for their preparation, and herbicides containing the above compounds.
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- Diacylium complexes of tetrahaloterephthalic acid
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Diacylium complexes of tetrahaloterephthalic acid can be produced by reacting tetrahaloterephthalic acid with sulfur trioxide to form compounds capable of reacting with various nucleophilics.
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