- A green disulfide synthesis method
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The present invention discloses a green disulfide synthesis method, belonging to the field of green chemical and organic synthesis technology. Under room temperature, open, neutral conditions, rapid preparation of parent nuclei is alkanes, olefins, aromatic hydrocarbons, oxazole, thiazole, pyrazole, imidazole, etc. and their derivatives of symmetrical disulfide, the catalyst is MBrx(M is Fe2+,Fe3+,Ce3+, etc., x is 2-3), the only oxidant isH2O2. The present invention is reacted by using commercially available and low-cost reagents (e.g., FeBr2,CeBr3 andH2O2,etc.) and common organic solvents, the steps are concise, the operation is convenient, the reaction is rapid, the reaction conditions are mild, the room temperature is open, and no further purification can be obtained pure disulfide, more advantageous than all previous methods, is expected to be in organic synthesis, medicine, Pesticides and electronics and other industries are widely used.
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Paragraph 0046-0048
(2022/01/08)
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- Electrochemical synthesis of organochalcogenides in aqueous medium
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The electrochemical preparation of telluride, selenide and sulfide ions was carried out in NaOH aqueous solution, using a two compartment cell. Organochalcogenides were prepared from halogenated compounds in a two-step procedure. The monochalcogenides were obtained as the major products in good yields.
- Ribeiro Neto, Pedro B.,Santana, Sonydelane O.,Levitre, Guillaume,Galdino, Danilo,Oliveira, Jadson L.,Ribeiro, Rogério T.,Barros, Maria E. S. B.,Bieber, Lothar W.,Menezes, Paulo H.,Navarro, Marcelo
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supporting information
p. 657 - 661
(2016/02/12)
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- Reaction mechanisms of thioetherification for mercaptans and olefins over sulfided Mo-Ni/Al2O3 catalysts
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The thioetherification reaction of 1-butanethiol and 1-hexene dissolved in n-hexane was investigatedover sulfided Mo-Ni/Al2O3catalysts. The experimental results showed the catalysts have good cat-alytic performance for thioetherification reaction, but the isomerization and hydrogenation reactions of olefins over the catalysts can inhibit thioetherification reaction. As reaction temperature increases,the isomerization and hydrogenation reactions of olefins increase rapidly, however, the inhibition of thioetherification reaction also increases. The sulfur distribution and molecular structures of sulfurcompounds in the products were analyzed by the gas chromatograph with sulfur chemiluminescencedetector (GC-SCD) and the gas chromatograph/mass spectra spectrometry (GC/MS). Two possible routesof thioetherification reaction could be observed. At low temperature, the major pathway involves a directaddition of 1-butanethiol to the terminal carbon of double bond of 1-hexene. In this mechanism, the mainproduct is anti-Markovnikov adduct. At a higher temperature, the C S bond of 1-butanethiol can be sub-sequently cleaved, and the adsorbed -SH species can be formed on the catalysts. On the same time,abundant 1-hexene can be absorbed on the catalysts, as well. Therefore, the adsorbed SH species canthen recombine with adsorbed 1-hexene to form new hexyl-mercaptans, which can continue to produceanother kind of thioether (di-hexyl sulfide) with adsorbed 1-hexene. Similar with the first reaction route,the thioether of the anti-Markonikov adduct still dominates in the product.
- Shen, Zhibing,Ke, Ming,Yu, Pei,Hu, Haiqiang,Song, Zhaozheng,Jiang, Qingzhe
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p. 120 - 127
(2015/02/02)
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- S-Acylation of aliphatic and aromatic thiols with carboxylic acids and their esters over solid acid catalysts in the gas phase at temperatures above 200 °c
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Benzenethiol is reacted with acetic acid in a hydrogen stream over [(Mo6Cl8)Cl4(H2O) 2]·6H2O. Catalytic activity of the clusters appears above 200 °C, yielding S-phenyl thioacetate. The selectivity is 98% at 300 °C. Niobium, tantalum, and tungsten halide clusters with the same octahedral metal framework also catalyze the reaction. Benzoic acid and aliphatic carboxylic acids afford the corresponding S-phenyl carbothioates by reaction with benzenethiol. Aliphatic thiols are also S-acylated to yield the corresponding S-alkyl carbothioates. When carboxylic esters are applied to the reaction with benzenethiol over [(Nb6Cl12)Cl 2(H2O)4]·4H2O at 450 °C, the sterically unhindered moiety of the ester is incorporated into the products: S-phenyl thioacetate or methyl phenyl sulfide is obtained selectively. A Br?nsted acid site developed on the cluster complex by thermal activation is the active site of the catalyst. Hence, solid acids such as silica-alumina, zeolites, and heteropoly acids that are stable above 200 °C also catalyze these reactions.
- Nagashima, Sayoko,Yamazaki, Hitomi,Kudo, Kentaro,Kamiguchi, Satoshi,Chihara, Teiji
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p. 332 - 338
(2013/07/26)
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- Microwave-assisted synthesis of disulfides using tetrathiomolybdate: A step toward greener synthesis
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An eco-friendly, efficient, and rapid synthetic procedure for disulfides using benzyl triethyl ammonium tetrathiomolybdate through microwave irradiation of solid support adsorbed reactants is reported.
- Sidiq, Naheed,Bhat, Mohsin Ahmad,Khan, Khaliquz Zaman,Khuroo, Mohammad Akbar
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experimental part
p. 373 - 376
(2012/08/28)
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- One-pot reduction of sulfoxides with NaBH4, CoCl2. 6H2O catalyst, and moist alumina
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Sulfoxides are reduced by a combination of sodium borohydride, a catalytic amount of cobalt(II) chloride hexahydrate, and chromatographic neutral alumina preloaded with a small amount of water (moist alumina) in hexane to produce the corresponding sulfides in good to excellent yields under mild conditions. An interesting structural influence of sulfoxides on their reactivity is observed. Copyright
- Yakabe, Shigetaka,Hirano, Masao,Morimoto, Takashi
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experimental part
p. 2251 - 2255
(2011/06/27)
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- METHOD FOR THE ORGANOMETALLIC PRODUCTION OF ORGANIC INTERMEDIATE PRODUCTS COMPRISING CARBON-HETEROATOM BONDS ACHIEVED BY THE DEPROTONATION OF HETEROATOMS
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The invention relates to a method for binding heteroatom-carbon bonds. According to said method, a lithium compound (II) is first generated by reacting aliphatic or aromatic halogen compounds (I) with lithium metal, said compound is then used for the deprotonation of the compounds (III) or (V). The lithium salts of formulas (IV) or (VI) obtained by said deprotonation are subsequently reacted with suitable carbon electrophiles (equation I), said process binding the heteroatom-carbon bond and forming the products (VIII) or (VIII), (equation I).
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Page/Page column 13
(2008/06/13)
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- Chemoselective deoxygenation of sulfoxides with titanium tetraiodide
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Chemoselective deoxygenation of sulfoxides was carried out using TiI4 as a reducing agent to give sulfides in good to excellent yields.
- Shimizu,Shibuya,Hayakawa
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p. 1437 - 1438
(2007/10/03)
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- Novel rearrangements of 2,3-dimercapto-1-propanol derivatives: Formation of dialkyl sulfide, dialkyl disulfide, and 1,2,3-tris(alkylthio)propane
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The base alkylation of 2,3-dimercapto-1-propanol with alkyl halides leads in good yield to 2,3-bis(alkylthio)-1-propanol and dialkyl sulfide. The reaction of 2,3-bis(alkylthio)-1-propanol with catalytic concentrated sulfuric acid proceeds with rearrangement to give 1,2,3-tris(alkylthio)propane and dialkyl disulfide. The rearrangement reaction takes place through a common intermediate thiaranium intermediate 8.
- Ong, Chi Wi,Chou, Yi Meen,Wang, Junn Nan
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p. 8244 - 8247
(2007/10/03)
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- METAL COMPLEX-CATALYZED SYNTHESIS OF DIHYDROTHIAPYRANS FROM DIALKYL SULFOXIDES AND 1,3-DIENES
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A preparative method has been developed for the synthesis of dihydrothiapyrans from dialkyl sulfoxides and 1,3-dienes, catalyzed by palladium and nickel complexes.The scope of this reaction has been assessed, and a mechanism proposed, using 1,3-dienes and sulfoxides of varying structure. Keywords: synthesis, dihydrothiapyrans, catalysts, mechanism, sulfides, 1,3-dienes.
- Dzhemilev, U. M.,Kunakova, R. V.,Baibulatova, N. Z.,Tarasenko, A. E.,Mustafina, E. M.
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p. 128 - 134
(2007/10/02)
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- Fluorodestannylation. A Powerful Technique to Liberate Anions of Oxygen, Sulfur, Selenium, and Carbon
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Fluoride ions smoothly destannylate organotin chalcogenides to liberate nucleophilic chalcogenide ions; hence the first nucleophilic oxide (O2-) and selenide (Se2-) transfer agents are reported where the tin atom serves as "group 16 (VIB) transfer agent".In the presence of crown ethers or ammonium salts, this process results in a new way to generate "naked" nucleophiles.Ethers and selenides are formed in good to excellent yield.In addition, a useful C-C bond-forming reaction has been developed by using alkyltins with aldehydes and acid chlorides in the presence of fluroide ion.Aspects concerning reactivity and mechanism are presented.Finally, the generality of the fluorodestannylation procedure and the differences with parallel silicon chemistry are detailed.
- Harpp, David N.,Gingras, Marc
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p. 7737 - 7745
(2007/10/02)
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- CYANO AND FLUORODESTANNYLATION: A NEW METHODOLOGY USING SOME POWERFUL SULFUR TRANSFER REAGENTS, THE ORGANOTIN SULFIDES
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Fluoride and cyanide ions destannylate bis(aralkyl)tin sulfides and trialkyltin sulfides giving, in the presence of a variety of alkyl and activated halides, the corresponding thioether derivatives in excellent yield.The conditions are mild, neutral and anhydrous; a strong solvent effect is noted.Special comments are made concerning work-up procedures.
- Harpp, David N.,Gingras, Marc
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p. 4373 - 4376
(2007/10/02)
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- UNE METHODE SIMPLE DE SYNTHESE DES PHOSPHATES TERPENIQUES ALLYLIQUES PRIMAIRES ET TERTIAIRES.
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Alkylation of tetrabutylammonium dihydrogenophosphate by terpenic allylic sulphonium salts give the corresponding primary terpenic allylic phosphates in fair to moderate yields, without complex procedures of purification.The catalysis of the reaction by cuprous ion leads to the isolation of tertiary allylic phosphates.
- Julia, M,Mestdagh, H.,Rolando, C.
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p. 3841 - 3850
(2007/10/02)
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- Determination of Sulfur in Asphalts by Selective Oxidation and Photoelectron Spectroscopy for Chemical Analysis
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The characterization of sulfur in asphalts is investigated by coupling selective reactions and photoelectron spectroscopy for chemical analysis.The specificity of the two following reactions has been studied on test compounds: oxidation of sulfides with tert-butyl hydroperoxide in chloroform (a); reduction by lithium aluminum hydride of sulfones in tetrahydrofuran (b).These reactions have been used with an asphalt, directly for (a) or after a preoxidation with m-chloroperbenzoic acid for (b) to determine, using photoelectron spectroscopy, which kind of sulfur was invol ved.An analytical scheme sums up the different results: cyclic sulfides = 67percent, thiophenic sulfides = 54percent, cyclanic sulfide = 13percent, alkyl and aryl alkyl sulfides = 33percent.
- Ruiz, Jean-Michel,Carden, Brian M.,Lena, Louis J.Vincent, Emile-Jean,Escalier, Jean-Claude
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p. 688 - 691
(2007/10/02)
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- REACTION OF SULFUR HALIDES WITH UNSATURATED COMPOUNDS XV. 2,2'-DICHLORO SULFIDES IN REACTION WITH ORGANOALUMINUM COMPOUNDS
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The reaction of 2,2'-dichloro sulfides with organoaluminum compounds was investigated.The reaction leads to dechlorination or alkylation products, depending on the structure of the organoaluminum compounds.It was established that nickel, titanium, and zirconium compounds have catalytic activity and enabled the reactions to occur under milder conditions.The addition of sulfur dichloride to 1-methyl- and 1,5-dimethyl-1,5-cyclooctadienes was investigated, and the rearrangement was followed in the series of 9-thiabicyclononane derivatives.
- Tolstikov, G. A.,Kantyukova, R. G.,Spirikhin, L. V.
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p. 1210 - 1218
(2007/10/02)
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