- A Schiff base bis(N-salicylidene)-3-oxapentane-1,5-diamine and its yttrium(III) complex: Synthesis, crystal structure, DNA-binding properties, and antioxidant activities
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A Schiff base bis(N-salicylidene)-3-oxapentane-1,5-diamine (H2L) and its yttrium(III) (Y(III)) complex, Y2L2(NO 3)2?2H2O, have been synthesized and characterized by physico-chemical and spectroscopic methods. The crystal structure of the Y(III) complex has been determined by single-crystal X-ray diffraction, revealing a centrosymmetric binuclear neutral entity where Y(III) centers are bridged by two phenoxo oxygens. The DNA-binding properties of the Schiff base H2L and the Y(III) complex were investigated by spectrophotometric methods and viscosity measurements. The results suggest that ligand H2L and Y(III) complex both bind to DNA via groove binding, and the Y(III) complex binds to DNA more strongly than H2L. The antioxidant activity of the Y(III) complex was determined by superoxide and hydroxyl radical-scavenging method in vitro, which indicates that Y(III) complex scavenges OH? and O2 radicals.
- Wu, Huilu,Pan, Guolong,Bai, Yuchen,Wang, Hua,Kong, Jin,Shi, Furong,Zhang, Yanhui,Wang, Xiaoli
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- A highly sensitive and selective fluorescent probe for Fe3+ based on 2-(2-hydroxyphenyl)benzothiazole
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A novel fluorescent Fe3+ probe (L)based on 2-(2-hydroxyphenyl) benzothiazole has been synthesized and characterized. Both UV-vis and fluorescence spectroscopic studies demonstrated that L was highly sensitive and selective towards Fe3+ over other metal ions in acetonitrile. Upon binding with Fe3+, the emission band of L red-shifted from 370 nm to 420 nm and the fluorescence intensity was enhanced ～103-fold. The lowest detection limit for L is 6.04 × 10-8 M and the dissociation constants Kd is 1.13 × 10-11 M, which were calculated from the fluorescence titration curves. The detailed UV-vis and fluorescent titrations studies suggested that the binding stoichiometry of the L-Fe3+ complex was 2:1, and the structure between L and the Fe 3+ complex was confirmed by the 1H NMR titration. Then IR spectra provided further proof of the binding mode of the L-Fe3+ complex.
- Liu, Shu-Di,Zhang, Liang-Wei,Liu, Xiang
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- A dichloro diethyl ether and 2 - chloroethyl phenoxy ethanol synthesis method
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The invention discloses a dichloro diethyl ether and 2 - chloroethyl phenoxy ethanol synthesis method, which belongs to the field of organic synthesis. The method comprises: the molar ratio of 0.8 - 1.5: 0.3 diethylene glycol and catalyst in a double-mouth flask, and the double-mouth flask are respectively connected with two of the mouth of the funnel and a condenser; the use of a separatory funnel to drip the mixed acid in double-mouth flask, in 130 °C - 170 °C under reaction, during the reaction, the use of condenser to collect condensate; the condensate to the distillation is carried out, to obtain dichloro diethyl ether; double-mouth flask in the remaining liquid to filter, to obtain the 2 - chloroethyl phenoxy ethanol, wherein mixed acid include: mass ratio is 25 - 35:1 of concentrated hydrochloric acid is concentrated sulfuric acid. The embodiment of the invention the synthesis method provided not only can at the same time obtained by synthesizing dichloro diethyl ether and 2 - chloroethyl phenoxy ethanol, but also, the method reaction is simple and controllable, mild reaction conditions, raw materials are safe and easily-obtained, so that the synthesis of the two more safe and controllable, the cost is cheaper.
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Paragraph 0061; 0065; 0070; 0075; 0081; 0092
(2019/05/16)
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- Preparation method of 4-dodecylphenol polyoxyethylene diether
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The invention relates to a preparation method of 4-dodecylphenol polyoxyethylene diether. The preparation method specifically comprises steps as follows: 1) synthesis of 2,2'-dichloroethyl ether; 2) synthesis of 4-dodecylphenol polyoxyethylene diether: 4-dodecylphenol, hexadecyl trimethyl ammonium bromide and 20% of a sodium hydroxide liquor are added to a four-neck flask, the mixture is stirred and heated, 2,2'-dichloroethyl ether is dropwise added to the four-neck flask within 1 h, and the mixture is rapidly heated for a reaction for 3-4 h, wherein the mass ratio of hexadecyl trimethyl ammonium bromide to 4-dodecylphenol is (1.2:10)-(5:10), and the mole ratio of 4-dodecylphenol to 2,2'-dichloroethyl ether is 2.02:1; after cooling, extraction is performed, a product is dried overnight, subjected to suction filtration and normal-pressure distillation for removal of a solvent, and a pasty product, namely, 4-dodecylphenol polyoxyethylene diether is obtained. The situation that synthesisof a dimeric surfactant long-branch diether intermediate mostly takes nonylphenol as a raw material is broken through.
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Page/Page column 6; 7
(2018/09/13)
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- Double (2-haloethyl) ether synthesis method
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The invention relates to the synthesis of fine chemical intermediates, in particular to a synthesis method of di(2-halogenated ethyl) ether. According to the synthesis method, 1,4-thioxane-1,1-dioxo and a hydrogen halide water solution react with each other to obtain the target product, namely di(2-halogenated ethyl) ether. The synthesis method is simple and convenient in technical route, good in selectivity, high in yield, less in pollution and simple in post-processing, conforms to the tendency of the green chemical industry nowadays, and has great industrial value.
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Paragraph 0020-0021
(2017/02/24)
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- A systematic study on the activation of simple polyethers by MoCl 5 and WCl6
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MoCl5, 1a, and WCl6, 1b, activate 1,3-dioxolane at room temperature in chlorinated solvents: the compound [MoOCl 3{OC(H)OCH2CH2Cl}]2, 2, has been isolated from MoCl5/dioxolane. The mixed oxo-chloro species WOCl 4, 1c, reacts with 1,3-dioxolane, selectively giving the coordination adduct WOCl4(κ1-C3H6O 2), 3. Dimethoxymethane, CH2(OMe)2, undergoes activation including C-H bond cleavage when reacted with 1a to give the molybdenum complexes [MoOCl3{OC(H)OMe}]2, 4, and Mo 2Cl5(OMe)5, 5. The reactions of 1b with CH 2(OR)2 (R = Me, Et) proceed via O-abstraction with formation of the oxo-derivatives WOCl4[O(R)CH2Cl] (R = Me, 6a; R = Et, 6b) in admixture with equimolar amounts of RCl. The reactions of 1a,b with CMe2(OMe)2 lead to mesityl oxide, MeC(O)CHC(Me)2. A series of simple diethers of general formula ROCH2(CHR′)OR′′ are activated by 1a,b in CDCl 3, usually via cleavage of C-O bonds at high temperature. The complex WCl5(OCH2CH2OMe), 7, has been detected in solution as an intermediate species in the course of the degradation of 1,2-dimethoxyethane (dme) by 1b. The activation of CH(OMe)3 by 1 is limited to C-O bonds and selectively gives methyl chloride and methylformate, which has been found coordinated in WOCl4[OC(H)OMe], 8. The organic fragments produced in the reactions have been detected by GC-MS and NMR analyses, upon hydrolysis of the reaction mixtures. Compounds 2 and 5, which have had their molecular structures ascertained by X-ray diffraction, represent rare examples of crystallographically-characterized dinuclear Mo(v) species containing both halides and oxygen ligands.
- Dolci, Sara,Marchetti, Fabio,Pampaloni, Guido,Zacchini, Stefano
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experimental part
p. 5367 - 5376
(2010/08/04)
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- Crosslinked polysaccharide, obtained by crosslinking with substituted polyethylene glycol, as superabsorbant
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New crosslinked polysaccharides useful as absorbents or superabsorbents alone or in a mixture are obtained by reacting polysaccharides (preferably containing carboxylates groups) with at least one crosslinker selected in the group constituted by activated polyethylene glycols such as for example halogenated (Cl, Br, I), mesylated, tosylated, or triflated activated polyethylene glycols.
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- A safe and efficient procedure to prepare alkyl and alkoxyalkyl chlorides and dichlorides by catalytic decomposition of the corresponding alkyl and alkoxyalkyl chloroformates and bischloroformates with hexabutylguanidinium chloride
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Small amounts of hexabutylguanidinium chloride (0.01 mol%) decomposes pure chloroformates or bischloroformates with different lengths of carbon chains by a semicontinuous process to diminish run-away risk, leading to chloride compounds with high yield and purity.
- Violleau,Thiebaud,Borredon,Le Gars
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p. 367 - 373
(2007/10/03)
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- The halogen-mediated opening of epoxides in the presence of pyridine-containing macrocycles
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The ring opening of epoxides with elemental iodine and bromine in the presence of three pyridine-containing macrocyclic diamides as new catalysts affords vicinal iodo alcohols and bromo alcohols in high yields. This new procedure occurs regioselectively under mild conditions in various aprotic solvents. The catalysts are easily recovered and can be reused several times.
- Sharghi, Hashem,Niknam, Khodabakhsh,Pooyan, Maryam
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p. 6057 - 6064
(2007/10/03)
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- 2-chloro-1,3-dimethylimidazolinium chloride. 3. Utility for chlorination, oxidation, reduction, and rearrangement reactions
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2-Chloro-1,3-dimethylimidazolinium chloride (1), which can act as a powerful dehydrating equivalent to DCC (2), is also applicable to chlorination, oxidation, reduction, and rearrangement under nearly neutral conditions. The utility of 1 for these reactions is described.
- Isobe, Toshio,Ishikawa, Tsutomu
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p. 5832 - 5835
(2007/10/03)
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- Synthese de Systemes Macromoleculaires a Caractere Complexant Derives de la 1,3-Dihydrobenzimidazole-2-thione
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Synthesis of macrocyclic compound by reaction between an ethylene glycol and the 1,n-bis(2-mercapto benzimidazolyl) di (and tri) ethylene glycol have been realised under phase transfer catalysis conditions.The compounds have been studied by proton nuclear magnetic resonance, mass spectrometry, infrared and by microanalysis.
- Zniber, Rachid,Regragui, Mohamed,Achour, Redouane,Cherkaoul, Omar,Hajji, Ahmed Jalal El,Cherkaoui, Mohammed Zoubair
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p. 457 - 462
(2007/10/03)
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- Metal-assisted Reactions. Part 17. Ring-opening and Dimerization of Cyclic Ethers by Titanium Halides
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Reaction of TiCl4 or TiBr4 with a variety of cyclic ethers gives, predominantly, products resulting from simple ring-opening or from ring-opening with simultaneous condensation to dimeric species.The variations in yields of these two kinds of products might be correlated qualitatively with an initial formation of the complex TiX4*2E (X = Cl or Br; E = cyclic ether) in which the ethers were held in a cis or trans relationship.Although such a correlation might suggest that TiCl4 but not TiBr4 exerts a template effect on the condensation, stereochemical considerations of the reaction products indicate otherwise.TiCl3 and VCl3 do not give similar results and TiF4 gives no reaction.
- Delaney, Paul A.,Johnstone, Robert A. W.,Entwistle, Ian D.
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p. 1855 - 1860
(2007/10/02)
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- STUDY OF THERMAL CONVERSIONS OF ETHYLENE CHLOROHYDRIN (2-CHLOROETHANOL).
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Ethylene chlorohydrin (ECH) is a widely used industrial solvent and reagent. When used at temperatures above 100-110 degree , ECH undergoes considerable decomposition. The authors of most publications, concerned with thermal stability of ECH, studied its hydrolysis in alkaline, acidic, and neutral solutions at temperatures up to 100 degree , and also free-radical decomposition of ECH at 430-496 degree in the gase phase. There is no information in the literature on the thermal stability of ECH in the liquid phase in the temperature range 110-150 degree . The purpose of the present work was to determine the principal relationships of thermal decomposition in anhydrous ECH in the liquid phase in the temperature range indicated above.
- Zil'berman,Kolesnikov,Danov,Efremov,Pantina
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p. 2344 - 2347
(2007/10/02)
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- NONAQUEOUS SOLUTION OF HYPOCHLOROUS ACID AND CHLOROHYDRINATION REACTIONS OF CERTAIN LOWER ALKENES.
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A study was made of the problems of preparing stable, highly concentrated nonaqueous solutions of hypochlorous acid and carrying out chlorohydrination reactions in them. The results on the chlorohydrination of alpha -alkenes showed that, in principle, it is possible and advisable to use solutions of hypochlorous acid in organic solvents, in particular, aliphatic and alicyclic ketones, ethyl acetate and tributyl phosphate. The use of organic solvents noticeably improves the stability of HOCl, so that the working concentrations of the acid can be increased, and the chlorohydrination reaction products can be more easily isolated.
- Bikbulatov,Valitov,Gromova,Stepanova,Martynova
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p. 2314 - 2317
(2007/10/02)
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- Process for preparing dimethylaminomethylenebis(phosphonic acid)
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Dimethylaminomethylenebis(phosphonic acid) is prepared by reacting dimethylformamide with phosphorous trichloride and treating the reaction mixture with alcohols or glycols and water. The phosphonic acid is combined with water soluble carboxylic acid polymers for use as a corrosion and scale inhibitor in aqueous systems. These compositions may also be combined with phosphorous acid and water soluble zinc salts.
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