Aryl sulfonyl fluoride synthesisviapalladium-catalyzed fluorosulfonylation of aryl thianthrenium salts
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Abstract:
We developed an efficient palladium-catalyzed fluorosulfonylation reaction of aryl thianthrenium salts to smoothly prepare various aryl sulfonyl fluorides using cheap Na2S2O4 as a convenient sulfonyl source in combination with N-fluorobenzenesulfonimide (NFSI) as an ideal fluorine source under mild reduction conditions. A one-pot synthesis of aryl sulfonyl fluorides starting from various arenes was established as well without the need for separating aryl thianthrenium salts. The practicality of this protocol was demonstrated by gram-scale synthesis, derivatization reactions, and excellent yields.Keywords:
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Monosaccharide
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Objective:On the base of the single factor investigation,response surface mathodology was applied to optimize the derivatization condition of taurolidine.Methods:Different derivatization reagent concentrations,reaction time and reaction temperature were taken as factor.The amount of the derivative products(expressed by peak area)was taken as response factor.Results:The optimizing derivatization condition of taurolidine was as follows:the reaction temperature(100 ℃),the derivatization reagent concentration(20 g·L-1),the reaction time(88 min).Conclusion:The method is accurate,reliable and can be applied to derivatize taurodiline.
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A new and rapid microwave assisted derivatization method for the determination of fatty acids in edible oil by GC MS was developed. The optimum conditions for derivatization, such as the derivatization solvent composition, microwave assisted derivatization pressure and time were studied for KOH methanol and H 2SO 4 methanol systems. The experimental results were compared with those obtained by traditional method of normal temperature derivatization .The applied range of the two derivatization systems was also discussed in detail. The derivatization was accomplished in 1 minute. Heptane was used as extraction solvent. The method is rapid, efficient, accurate and solvent saving.
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Synthesis of 2-amino-4-aryl-5-arylsulfonyl thiazoles 2a-i have been successfully carried out in one pot by condensing α-aryl sulfonyl-4-substituted acetophenones with phenyl trimethyl ammonium tribromide (PTT) and thiourea. The required α-aryl sulfonyl-4-substituted acetophenones have also been prepared by modified one pot method.
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This survey gives an overview of recent derivatization protocols, starting from 1996, in combination with capillary electrophoresis (CE). Derivatization is mainly used for enhancing the detection sensitivity of CE, especially in combination with laser-induced fluorescence. Derivatization procedures are classified in tables in pre-, on- and postcapillary arrangements and, more specifically, arranged into functional groups being derivatized. The amine and reducing ends of saccharides are reported most frequently, but examples are also given for derivatization of thiols, hydroxyl, carboxylic, and carbonyl groups, and inorganic ions. Other reasons for derivatization concern indirect chiral separations, enhancing electrospray characteristics, or incorporation of a suitable charge into the analytes. Special attention is paid to the increasing field of research using on-line precapillary derivatization with CE and microdialysis for in vivo monitoring of neurotransmitter concentrations. The on-capillary derivatization can be divided in several approaches, such as the at-inlet, zone-passing and throughout method. The postcapillary mode is represented by gap designs, and membrane reactors, but especially the combination of separation, derivatization and detection on a chip is a new emerging field of research. This review, which can be seen as a sequel to our earlier reported review covering the years 1991—1995, gives an impression of current derivatization applications and highlights new developments in this field.
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An efficient and highly regioselective synthesis of 1-allenyl-5-aryl-1,2,3-triazoles from 1-sulfonyl-4-aryl-1,2,3-triazoles is disclosed. 1-Sulfonyl-4-aryl-1,2,3-triazoles reacted with propargylic alcohols in the presence of trifluoroboron etherate to furnish 1-allenyl-5-aryl-1,2,3-triazoles. When secondary alcohols were used as substrate, the outcome of the reaction was 1-alkyl-5-aryl-1,2,3-triazoles.
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