- Concentration of hydrophobic organic compounds and extraction of protein using alkylammoniosulfate zwitterionic surfactant mediated phase separations (cloud point extractions)
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The zwitterionic surfactants 3-[nonyl- (or decyl-) dimethylammonio]propyl sulfate, (C9-APSO4 or C10-APSO4) were synthesized using Nilsson's procedure, and their phase separation behavior under different experimental conditions was evaluated. The results indicate that such zwitterionic surfactants can be utilized for the extraction/preconcentration of hydrophobic species in a manner akin to that previously reported for nonionic surfactants. This was demonstrated for several practical applications including the extraction/preconcentration of some steroidal hormones and vitamin E prior to high-performance liquid chromatography analysis. The zwitterionic surfactant mediated phase separation was also applied to the extraction of the hydrophobic membrane protein, bacterio-rhodopsin, from the hydrophilic cytochrome c protein, both originally present In an aqueous phase. The concentration factors for this aqueous two-phase extraction technique using C10-APSO4 ranged from 26 to 35 with recoveries In the range 88 to > 96%. Some comparative studies Indicate that the use of zwittterionic surfactants In lieu of nonionic surfactants (e.g. polyoxyethylene(7.5) nonyl phenyl ether PONPE-7.5) In such an extraction method offers some significant advantages such as purer, homogeneous surfactant preparation, minimum background absorbance at UV detection wavelengths, the two-phase region occurring at lower temperatures, and greater extraction efficiencies/concentration factors among others.
- Saitoh, Tohru,Hinze, Willie L.
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- METHOD OF OXIDIZING USING CALCIUM HYPOCHLORIDE AND MANUFACTURING FOR SULFONE OR SULFIDE
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Is a process for preparing a sulphone or sulfate compound using calcium hypochlorite, and, wherein the method comprises introducing, sulfoxide or sulfite compound in an organic solvent and adding calcium hypochlorite in a solid state to an organic solvent in which the compound is introduced to oxidize the compound. (by machine translation)
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Paragraph 0111-0114; 0116; 0117; 0131
(2020/06/11)
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- Preparation method of propylene sulfate
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The invention discloses a preparation method of propylene sulfate, belonging to the field of preparation of lithium ion battery additives. The preparation method of the propylene sulfate comprises thefollowing steps: with chlorosulfonic acid and 1,3-propylene glycol as raw materials, preparing an intermediate (3-hydroxypropoxy)sulfonic acid at first; and carrying out an intramolecular dehydrationcyclization reaction on the intermediate (3-hydroxypropoxy)sulfonic acid to obtain the propylene sulfate. The raw materials for synthesizing the propylene sulfate are easy to obtain, operation process is simple and safe, product yield is high, and a production period is short; no wastewater or waste salt is generated in the process of synthesizing the propylene sulfate; a catalyst and a solvent with water can be recycled, and special equipment is not needed; and the method is suitable for industrial application.
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Paragraph 0056-0077
(2020/06/16)
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- Sulfate preparation method
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The invention relates to the field of organic synthesis, and especially relates to a sulfate preparation method. The invention provides a sulfate preparation method. According to the preparation method, a compound represented by a formula (II) reacts with sulfuryl fluoride in the presence of a reaction solvent to prepare a compound represented by a formula (I). During the sulfate preparation process, the introduction of water and chlorine ions is avoided effectively, the situation that the product is degraded and the chlorine ion content is high is avoided therefore; moreover, the steps of thepreparation method are simple and short, the raw material are common chemical products on the market, the kinds of raw materials and the side reactions are few, and the yield is high. The manufacturing cost is low, only recyclable organic solvents are used, the reaction byproduct is a single inorganic salt solid and can be easily recovered, no wastewater is generated, the environment is better protected, and the sulfate preparation method is green and environmentally friendly and is suitable for industrial large scale production.
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Paragraph 0074; 0075; 0076; 0077
(2018/09/11)
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- Preparation method of cyclic sulfate
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The invention relates to the field of organic synthesis, in particular to a preparation method of cyclic sulfate. The structural formula of cyclic sulfate is shown as formula I. The preparation methodof cyclic sulfate comprises the following step: cyclic sulfate in the formula I is prepared from a compound in formula II and sulfuryl fluoride by reacting in the presence of an acid binding agent and a catalyst. The preparation method of cyclic sulfate adopts short reaction step, cyclic sulfate can be prepared with the one-step reaction, cost of raw and auxiliary materials is low, and expensiveraw materials and oxidizing agent are not used.
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Paragraph 0086; 0087; 0088; 0089; 0090
(2018/03/28)
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- Cyclic sulphate preparation method
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The invention relates to the field of organic synthesis and especially relates to a cyclic sulphate preparation method. The sulphate preparation method disclosed by the invention comprises the step ofreacting a compound shown in formula II with sulfuryl chloride under the reaction solvent existence condition to prepare and obtain a compound shown in formula I. The sulphate preparation method disclosed by the invention has the characteristics of brief steps, small side reaction, simpleness in aftertreatment, small three wastes, low manufacturing cost, suitability for industrial large-scale production and the like.
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Paragraph 0079; 0080; 0081; 0082
(2018/09/11)
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- Synthesis and biological evaluation of deoxy salacinols, the role of polar substituents in the side chain on the α-glucosidase inhibitory activity
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Three analogs (5, 6, and 7) lacking polar substituents in the side chain of a naturally occurring α-glucosidase inhibitor, salacinol (1a), were synthesized by the coupling reaction of a thiosugar, 1,4-dideoxy-1,4-epithio-d- arabinitol (3), with cyclic sulfates (8, 9, and 10), and their α-glucosidase inhibitory activities were examined. All these simpler analogs (5, 6, and 7) showed less inhibitory activity compared to 1a, and proved the importance of cooperative role of the polar substituents for the α-glucosidase inhibitory activity. A practical synthetic route to 3 starting from d-xylose is also described.
- Muraoka, Osamu,Yoshikai, Kazuya,Takahashi, Hideo,Minematsu, Toshie,Lu, Guangxin,Tanabe, Genzoh,Wang, Tao,Matsuda, Hisashi,Yoshikawa, Masayuki
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p. 500 - 509
(2007/10/03)
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- Substituted isoquinolines as ultra short acting neuromuscular blockers
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Ultra short acting neuromuscular blocking agents of Formula (I) which are useful as skeletal muscle relaxants during emergency intubation procedures, routine surgery and post-operative settings are disclosed, wherein q and t are independently from 0 to 4; X1 and X2 are independently halogen; ha and hb are independenity from 0 to 2; Z1 and Z2 are indepentdently hydrogen, C1-6 alkyl, C2-6 alkenyl or C2-6 alkynyl with the proviso that Z1 and Z2 are not both hydrogen; Y1, Y2, and Y3 and Y4 are independently hydrogen, halogen or C1-3 alkoxy; m and p are independently 1 to 6; n and r are independently 0 to 4; with the proviso the if ha and hb are both 0, then r is 0 and n is 0 to 2; R1 to R14 are independently hydrogen, halogen, C1-3 alkoxy, or R2 and R3 together with the carbon atoms to which they are bonded, R5 and R6 together with the carbon atoms to which they are bonded, R9 and R10 together with the carbon atoms to which they are bonded, R12 and R13 together with the carbon atoms to which they are bonded, may independently form a methylenedioxy or ethylenedioxy moiety contained in five- or six-membered ring; W1 and W2 are carbon; and A is a pharmaceutically acceptable anion.
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- Synthesis of Ultra-Short-Acting Neuromuscular Blocker GW 0430: A Remarkably Stereo- and Regioselective Synthesis of Mixed Tetrahydroisoquinolinium Chlorofumarates
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(Matrix Presented) The stereo- and regioselective synthesis of ultra-short-acting nondepolarizing neuromuscular blocker GW 0430 (5a) is de scribed. Key steps involved the enantioselective transfer hyrogenation of imine 8 employing Noyori's catalyst, the stereoselective catallization and methanolysis of trans-betains 11 and 12, and the stereo- and regioselective trans elimination of hydrogen chloride 'from 14. The latter transformation allowed complete control of the position of the chloro substituent and stereochemistry at the double bond of the linker in 15.
- Samano, Vicente,Ray, John A.,Thompson, James B.,Mook Jr., Robert A.,Jung, David K.,Koble, Cecilia S.,Martin, Michael T.,Bigham, Eric C.,Regitz, Craig S.,Feldman, Paul L.,Boros, Eric E.
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p. 1993 - 1996
(2008/02/11)
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- A new route for the synthesis of amphiphilic and water-soluble ligands: Monoand di-tertiary phosphines having an alkylene sulfate chain
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Cyclic sulfates react with LiPPh2 to form a series of new amphiphilic or water-soluble ligands: monotertiary phosphines with one or two alkylene sulfate chains and ditertiary phosphines with one or two hydrophilic tails attached to bridgehead carbon atom; the application of zwitterionic RhI complexes (sulfatephos)2Rh(cod) and (sulfatediphos)Rh(cod) in liquid biphasic catalysis has been demonstrated for the hydroformylation of styrene and oct-1-ene.
- Gulyas, Henrik,Arva, Peter,Bakos, Jozsef
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p. 2385 - 2386
(2007/10/03)
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- Direct transformation of dialkyl sulfates into alkyllithium reagents by a naphthalene-catalysed lithiation
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The lithiation of primary and secondary dialkyl sufates with an excess of lithium powder in the presence of a catalytic amount of naphthalene (4 mol %) in THF at -78°C leads to the corresponding alkyllithium reagents (1:2 molar ratio) which react with different electrophiles, mainly carbonyl compounds, to yield after hydrolysis, the expected coupling products. This methodology represents an indirect way to transform alcohols into organolithium compounds through the corresponding dialkyl sulfates. When the same procedure is applied to five or six member cyclic sulfates (derived from 1,2- or 1,3-diols) only products arising from a β- or γ-elimination process (giving olefins or cyclopropanes), respectively, are obtained.
- Guijarro, David,Guillena, Gabricia,Mancheno, Balbino,Yus, Miguel
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p. 3427 - 3436
(2007/10/02)
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- ELECTROCHEMICAL REDUCTION OF CYCLIC AND ACYCLIC SULFATES.
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It was confirmed that cyclic and acyclic sulfates of diols and monoalcohols could be reduced at cathodes in nonaqueous solvents. The reduction products were greatly affected by the molecular structures of the sulfates. The reduction of the cyclic sulfates of 1,2-diols yielded the corresponding alkenes and disulfate dianions of the parent diols in high yields and current efficiencies were based on one-electron reduction. On the other hand, the cyclic sulfates of 1,3- and 1,4-diols were also reduced by one-electron transfer under similar conditions, but the cycloalkanes expected were not formed and the products were cyclic ethers along with acyclic alkane or unsaturated alcohol. The reduction of the cyclic sulfate of hydrated formaldehyde, which is regarded as a 1,1-diol, did not give any identified products except for a small amount of methane.
- Nonaka,Kihara,Fuchigami,Baizer
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p. 3160 - 3166
(2007/10/02)
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- Application of a Lanthanide Shift Reagent in 17O N.M.R. Spectroscopy to determine the Stereochemical Course of Oxidation of Cyclic Sulphite Diesters to Cyclic Sulphate Diesters with Ruthenium Tetroxide
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Cyclic sulphite diesters are rapidly oxidized to cyclic sulphate diesters with ruthenium tetroxide in good yield; diastereotopically labelled cyclic sulphate diesters obtained by oxidation of diastereoisomeric cyclic sulphite diesters with ruthenium tetroxide are shown, by the effect of a lanthanide shift reagent on their 17O n.m.r. signals, to be formed with retention of configuration at sulphur.
- Lowe, Gordon,Salamone, Salvatore J.
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p. 1392 - 1394
(2007/10/02)
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