- Redox-Active 1D Coordination Polymers of Iron-Sulfur Clusters
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Here we describe the combination of an archetypal redox-active metal sulfide cluster, Fe4S4, with an organic linker, 1,4-benzenedithiolate, to prepare coordination polymers containing infinite chains of Fe4S4 cl
- Horwitz, Noah E.,Xie, Jiaze,Filatov, Alexander S.,Papoular, Robert J.,Shepard, William E.,Zee, David Z.,Grahn, Mia P.,Gilder, Chloe,Anderson, John S.
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- Preparation method of p-dithiophenol
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The invention discloses a preparation method of p-dithiophenol, wherein the p-dithiophenol is directly synthesized from p-dichlorobenzene and sodium hydrosulfide under a reaction of a catalyst. The p-dithiophenol obtained by the preparation method disclos
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Paragraph 0027-0043
(2020/04/22)
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- Method for preparing sulfhydryl compounds by hydroxyl substitution and sulfhydryl compounds
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The invention provides a method for preparing sulfhydryl compounds by hydroxyl substitution and the sulfhydryl compounds. According to the method, low-cost and easily-obtained benzene or fused ring compounds with phenolic hydroxyl groups or benzyl hydroxyl substituents serving as raw materials to react with the raw materials such as inorganic sulfide under the catalysis conditions to prepare the corresponding sulfhydryl compounds. The method has the advantages that the preparation method is simple, convenient and rapid, low in cost, mild in reaction condition, high in reaction site selectivity and high in yield, a post-processing process is simple, and no pollution is caused.
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Paragraph 0055; 0056; 0057; 0064; 0065; 0066
(2017/06/02)
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- Synthetic method for 1,4-dithioalkyl benzene and halide thereof
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The invention relates to a synthetic method for 1,4-dithioalkyl benzene and halide thereof. According to the method, 4-bromothiophenol is used as a raw material and reacts with alkyl bromide to synthesize 4-bromo-1-thioalkyl benzene, and then a reaction is carried out to synthesize 1,4-dithioalkyl benzene; or 4-bromothiophenol successively reacts with n-butyl lithium, sulfur powder and acid to synthesize 1,4-benzenedithiol, and then1,4-benzenedithiol reacts with alkyl bromide to synthesize 1,4-dithioalkyl benzene; and 1,4-dithioalkyl benzene can be further halogenated. The synthetic method provided by the invention does not need flammable and combustible t-butyl lithium, so the synthetic method has better security and controllability, is favorable for large-scale industrial production, reduces production cost and is environment friendly.
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Paragraph 0019; 0020; 0021; 0022; 0023
(2017/03/08)
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- MALDI-TOF/TOF CID study of poly(p-phenylene sulfide) fragmentation reactions
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A study involving the evaporation-grinding MALDI sample preparation method, MALDITOF/TOF CID, and Py-GC/MS is presented to examine the fragmentation mechanisms of poly(p-phenylene sulfide) (PPS). MALDI-TOF/TOF CID fragmentation studies yielded a wealth of information about the mass, structure (linear or cyclic), end-groups, and backbone modifications of the polymer. Additionally, Py-GC/MS experimental data are presented for comparison of the multimolecular free radical reactions in pyrolysis with the unimolecular fragmentation reactions of MS/MS.1,2 TOF/TOF CID results indicate that linear PPS undergoes random main chain fragmentation along the polymer backbone and preferentially fragments at bonds adjacent to dibenzothiophene and phenyl end-groups. Cyclic species produce fragment ions similar to linear species. However, the MS/MS precursor ions for cyclic PPS are, by far, the most intense peaks, while the precursor ions for linear species show relatively low intensity. CID fragmentation results are supported by Py-GC/MS data and are consistent with the proposed degradation mechanisms.
- Gies, Anthony P.,Geibel, Jon F.,Hercules, David M.
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experimental part
p. 952 - 967
(2011/10/08)
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- Process for preparation of aromatic thiols
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Disclosed is a process for preparation of an aromatic thiol corresponding to the structure wherein A is a substituted or unsubstituted aromatic radical and n is 1, 2, 3, 4, 5 or 6 comprising contacting at a temperature of at least 80° C. an aromatic halide corresponding to the structure wherein A is the same as above, X is bromine or iodine and n is 1, 2, 3, 4, 5, or 6 with thiourea in the presence of nickel metal.
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- HIGH-TEMPERATURE ORGANIC SYNTHESIS. XLI. REACTIONS OF AROMATIC HALOGEN COMPOUNDS WITH HYDROGEN SULFIDE IN THE PRESENCE OF SULFUR
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The reactions of halogenoarenes containing a sufficiently mobile halogen atom with hydrogen sulfide in the presence of elemental sulfur at 90-230 deg C lead to the corresponding sulfides (with yields of up to 87percent).The disulfides, thiols, and arenes are formed at the same time.In the reactions of bromophenols with hydrogen sulfide in the presence of sulfur migration of the halogen atom is observed, and this leads to the formation of isomeric bis(hydroxyphenyl) sulfides and disulfides and 2,4-dibromophenol.It was established that the yield of the reaction products depends on the time, temperature, halogenophenol-sulfur ratio, and delivery rate of hydrogen sulfide.The radical mechanism of the formation of these substances is discussed.
- Papernaya, L. K.,Panova, G. M.,Deryagina, E. N.,Voronkov, M. G.
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p. 1856 - 1862
(2007/10/02)
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- Spectra, Ionization Constants, and Rates of Oxidation of 1,4-Dimercaptobenzene and Properties of the p-Mercaptophenylthiyl and p-Benzodithiyl Anion Radicals
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In basic solution, p-dimercaptobenzene, which is found to have pKa's of 6.0 and 7.7, is rapidly oxidized by azide radical (k = 7.4*109 M-1 s-1) to p-benzodithiyl radical anion, the sulfur analog of p-benzosemiqu
- Armstrong, D. A.,Sun, Qun,Tripathi, G. N. R.,Schuler, R. H.,McKinnon, D.
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p. 5611 - 5617
(2007/10/02)
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- THE REACTION BETWEEN ARENEDIAZONIUM TETRAFLUOROBORATES AND ALKALINE THICARBOXYLATES IN DMSO: A CONVENIENT ACCESS TO ARYL THIOLESTERS AND OTHER AROMATIC SULFUR DERIVATIVES.
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The reaction between potassium thioacetate or sodium thiobenzoate and arenediazonium tetrafluoroborates in DMSO leads to the corresponding aryl thiolesters 1 which can either be isolated or further reacted providing a convenient one-pot access to a number of other aromatic sulfur derivatives.
- Petrillo, Giovanni,Novi, Marino,Garbarino, Giacomo,Filiberti, Marcos
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p. 7411 - 7420
(2007/10/02)
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- SYNTHESIS OF AROMATIC THIOLS FROM ARYL IODIDES AND THIOUREA BY MEANS OF NICKEL CATALYST
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Nickel(0) complex, generated in situ from bis(triethylphosphine)nickel(II) chloride and sodium cyanoborohydride, catalyzed the nucleophilic displacement of aryl iodides with thiourea.S-Aryl-isothiuronium salts or aromatic thiols were obtained in good yields after simple work-up procedures.
- Takagi, Kentaro
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p. 1307 - 1308
(2007/10/02)
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- SELECTIVE DEALKYLATIONS OF ARYL ALKYL ETHERS AND THIOETHERS BY SODIUM IN HMPA
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The reaction of sodium with bis- and tris(alkoxy)benzenes in HMPA gives selectively the products of monodealkylation.The reaction proceeds through a dianion which fragments into an alkyl and an aryloxy anion.The positional selectivity of this fragmentation is governed by the structure of both the alkyl and aryloxy groups.With bis- and tris(alkoxy)benzenes which for symmetry reasons can afford aryloxy anions having the same basicity, the dealkylation involves exlusively the less substituted alkyl group.On the contrary, in the asymmetric terms, the positional selectivity of the dealkylation process is governed by the basicity of the aryloxy anion.On the basis of these concepts several efficient and synthetically useful reactions have been developed.In most cases the selectivity obtained in the present reactions in different from that observed with other previously developed methods which use sodium methoxide or sodium alkenethiolates in HMPA.It is shown that the appropriate choice of the reagent allows selective dealkylation of the desired alkoxy group of a poly(alkoxy)benzene.The reaction of sodium with bis(alkylthio)benzenes in HMPA gives the bis(mercapto)benzenes.If the reduction is carried out with a solution of sodium in HMPA, the reaction gives instead the products of monodealkylation.This however is not selective.It is suggested that in the case of thioethers the dealkylation products originate from the fragmentation of the radical anions.
- Testaferri, L.,Tiecco, M.,Tingoli, M.,Chianelli, D.,Montanucci, M.
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p. 3687 - 3692
(2007/10/02)
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- Fragmentation of Aryl Alkyl Sulfides. A Simple, One-Pot Synthesis of Polymercaptobenzenes from Polychlorobenzenes
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A simple procedure is described which allows one to prepare polymercaptobenzenes starting from chlorobenzenes.The reactions of all the possible chlorobenzenes with Me2CHSNa in HMPA give the corresponding (isopropylthio)benzenes which can be cleaved by adding sodium to the reaction mixtures to give the arenethiolates in good yields.In some cases the polymercaptobenzenes were isolated after treatment with acid; in other cases methyl iodide was added to the reaction mixture and poly(methylthio)benzenes were obtained.It is suggested that the (isopropylthio)benzenes react with sodium to give the corresponding radical anions which fragment at the sulfur-alkyl bond to give the arenethiolates.
- Maiolo, Filippo,Testaferri, Lorenzo,Tiecco, Marcello,Tingoli, Marco
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p. 3070 - 3073
(2007/10/02)
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