Although many electrophilic trifluoromethylating agents have been reported to date, practically useful reagents have yet to be developed. S-(Trifluoromethyl)dibenzothiophenium salts, known as Umemoto's reagents, have two significant drawbacks that have hampered their practical application: (1) synthesis involving many steps and (2) the formation of large amounts of dibenzothiophene as waste after trifluoromethylation. Our idea to substitute fluorine at specific positions on the dibenzothiophenium rings has resulted in massive improvements in the synthesis, properties, reactivity, and applications of these compounds. On the basis of this idea, 2,8-difluoro- and 2,3,7,8-tetrafluoro-S-(trifluoromethyl)dibenzothiophenium triflates and other salts were developed as powerful, thermally stable, one-pot-preparable, and recyclable reagents for the trifluoromethylation of various types of nucleophilic substrates, such as carbanions, (hetero)aromatics, alkenes, alkynes, thiols, sulfinates, and phosphines. This one-pot and recycled production tremendously decreases the chemical and environmental costs of this process. Because of their higher reactivity and thermal stability, these new reagents may have wider applications than Umemoto's reagents. Therefore, these new versions of Umemoto's reagents could be widely used as the first practically useful electrophilic trifluoromethylating agents for the production of many types of trifluoromethyl-containing compounds in academic and industrial applications.
In this work, a simple and fast sample pretreatment method was proposed for determination of steroid hormones in fish tissues by coupling dynamic microwave-assisted extraction with salting-out liquid-liquid extraction. The steroid hormones were successively extracted with acetonitrile and water under the action of microwave energy. Subsequently, the extract was separated into an acetonitrile phase and an aqueous phase with ammonium acetate. The acetonitrile phase containing the target analytes was concentrated and determined by LC-MS/MS. The limits of detection for the steroid hormones were in the range of 0.03-0.15 ng g(-1). This method was successfully applied to analyze seven kinds of fish tissues, and the recoveries of the steroid hormones for the spiked samples were in the range of 75.3 ± 4.9% to 95.4 ± 6.2%. Compared with the traditional method, the proposed method could reduce the consumption of the organic solvent, shorten the sample preparation time, and increase the sample throughput.
A robust dearomative denitration of nitroarene derivatives induced by radical ipso-cyclization process has been developed, delivering valuable phosphonated or trifluoromethylated azaspiro[4.5]trienones with good functional group tolerance. It demonstrated a convenient...
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