- Synthetic method of 1-(2-fluorophenyl)-1-(4-fluorophenyl)ethylene oxide
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The invention discloses a synthetic method of 1-(2-fluorophenyl)-1-(4-fluorophenyl)ethylene oxide, comprising the following steps: firstly mixing 1-bromo-n-decane and sodium methyl mercaptide, addingtetrabutylammonium bromide and carrying out a reaction, and conducting aftertreatment on the reaction product so as to obtain n-decyl methyl sulfide; dissolving n-decyl methyl sulfide and dimethyl sulfate in a solvent I, and carrying out a heating reflux reaction; carrying out reduced pressure distillation of the solvent I after the reaction so as to obtain a reaction product containing sulfoniumsalt; carrying out an epoxidation reaction by successively adding the reaction product containing sulfonium salt, sodium hydroxide and 2,4'-difluorobenzophenone into a solvent II, and carrying out aftertreatment after the reaction so as to obtain 1-(2-fluorophenyl)-1-(4-fluorophenyl)ethylene oxide. By the method for synthesizing 1-(2-fluorophenyl)-1-(4-fluorophenyl)ethylene oxide, the invention has technical advantages of environmental protection, high yield and the like.
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Paragraph 0030-0032; 0037-0039
(2019/01/21)
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- Sulfonium salt type chloramine antibacterial agent and synthetic method thereof
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The invention belongs to the technical field of chemical synthesis and application of chloramine antibacterial agents, and provides a sulfonium salt type chloramine antibacterial agent and a syntheticmethod thereof. A preparation method of the antibacterial agent comprises the following steps: taking bromoalkyl 5,5-dimethylhydantoin and thioether as raw materials to prepare a sulfonium salt bromide chloramine precursor compound IV; reacting the precursor compound IV with t-butyl hypochlorite at normal temperature after ion exchange to obtain an antibacterial agent compound I. The antibacterial agent disclosed by the invention introduces a cationic structural unit-sulfonium salt group into a hydrophobic chain chloramine group, so that water solubility of the chloramine antibacterial agentis greatly improved and structure stability of the chloramine antibacterial agent is significantly enhanced. By using staphylococcus aureus as a model strain, the antibacterial test result shows thatthe bactericidal activity of the prepared sulfonium salt type chloramine compound is better than that of a mono-quaternary ammonium salt type chloramine compound.
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Paragraph 0047; 0048
(2018/11/22)
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- Ex Situ Formation of Methanethiol: Application in the Gold(I)-Promoted Anti-Markovnikov Hydrothiolation of Olefins
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A protocol for the Au-promoted anti-Markovnikov hydrothiolation of olefins using ex situ generated methanethiol is reported. The use of S-methylisothiourea hemisulfate salt as a solid precursor for methanethiol generation ensures a safe and reliable deliverance of a stoichiometric amount of this thiol. The procedure was shown to work for a broad range of olefins providing the corresponding hydrothiolated adduct in good to excellent yields. Mechanistic evaluations suggest that thiyl radicals are generated and that gold acts as an efficient but stable radical initiator.
- Kristensen, Steffan K.,Laursen, Simon L. R.,Taarning, Esben,Skrydstrup, Troels
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supporting information
p. 13887 - 13891
(2018/10/02)
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- Effect of the presence of ionic liquid during the NiMoS bulk preparation in the transformation of decanoic acid
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The impact of the presence and amount of [BMIM][NTf2] ionic liquid during the preparation of bulk NiMoS catalysts was investigated. It was clearly shown that these factors have a strong influence on both the morphology and specific surface area of the obtained NiMoS samples. Most interestingly the catalytic activity for the transformation of decanoic acid increased up to three times when IL was present during synthesis. In the same time, a greater selectivity towards hydrocarbons was observed. On the whole a clear relationship between catalytic activity, selectivity and NiMoS morphology was demonstrated. Consequently, it is possible to modify the morphology of the materials and impact the catalytic properties by changing the synthesis conditions.
- Leyral, Géraldine,Brillouet, Soizic,Rousseau, Julie,Richard, Frédéric,Mamede, Anne Sophie,Courthéoux, Laurence,Pradel, Annie,Ribes, Michel,Brunet, Sylvette
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p. 120 - 132
(2017/01/11)
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- Methyl transfers. 14. Nucleophilic catalysis of nucleophilic substitution
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Nucleophiles X- can catalyze the substitution Nu- + RY → NuR + Y- by adding the faster pathway X- + RY → XR + Y- followed by Nu- + XR → RNu + X-. New examples include catalysis by I- of the exchange of methyl between two dialkyl sulfides and the transfer of methyl from an arsonium salt to a phosphine. The individual reactions are separately studied and some equilibrium information is presented. Iodide is ineffective in the transfer of methyl between two pnosphines, which is not detected with or without iodide. The Marcus equation treatment of this catalysis is shown to require that the identity transfer of R between two X- groups be far faster than that for transfer of R between two Nu- groups. Nucleophiles other than I- are discussed. The possibility that some "supernucleophiles" may have fast identity rates is discussed, and literature evidence that this is indeed the case is presented. Stereochemical studies using chiral methyl derivatives have shown that vitamin B12 does provide a nucleophilic catalysis to methyl transfer in living systems. Thus, the apparently superfluous participation of B12 in some biological methyl transfers is explained.
- McCortney,Jacobson,Vreeke,Lewis
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p. 3554 - 3559
(2007/10/02)
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- The Preparation of (Methylthio)- and (Methylseleno)-tri(alkyl or aryl)phosphonium Salts and Their Reactions with Carboxylic Acids and Alcohols
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A series of (methylthio)- and (methylseleno)-triphenylphosphonium salts and the analogous tributylphosphonium salts have been prepared by methylation of the corresponding tertiary phosphine sulfides and selenides.Details of their 1H, 13C and 31P n.m.r. spectra are given.Whereas the (methylthio)- and (methylseleno)-triphenylphosphonium salts undergo rapid decomposition in the presence of tertiary ammonium carboxylates or tertiary amines, the (methylthio)- and (methylseleno)-tributylphosphonium salts convert such carboxylates into methanethiol and methaneselenol estersin acceptable yields.A tris(dimethylamino)(methylthio)phosphonium salt, on the other hand, converts benzoate into methyl benzoate in quantitative yield.Inferior yields of (methylthio)- and (methylseleno)-alkanes are obtained from two primary alcohols and the tributylphosphonium salts.
- Haynes, Richard K.,Indorato, Carlo
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p. 1183 - 1194
(2007/10/02)
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