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A serendipitiously discovered, extremely simple, fast and previously unreported method for the preparation of symmetrical aliphatic, aromatic and heteroaromatic disulfides is reported. Addition of sulfuryl chloride to an alkyl- or arylthiol in a 1:2 ratio under solvent free conditions or in dichloromethane solution produces the corresponding disulfides in nearly quantitative yields with the concomitant elimination of gaseous SO2 and 2 equiv of HCl. Thus, optimally the reaction needs no work-up at all leaving the disulfide as the sole product in excellent yield. In dichloromethane solution, the reaction is conveniently carried out in a rotary evaporator by mixing the solvent, thiol and SO2Cl2 in a round-bottomed flask followed by evaporation of the volatiles.  相似文献   

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A new, faster and cleaner method for the synthesis of heterobimetallic alkyne complexes is reported. Higher yields than previously obtained are achieved and in some cases moderate stereoselectivity has also been observed.  相似文献   

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While excellent methods exist for the oxidation of sulfides to sulfoxides R1R2S-->R1R2SO, the azaversion of this atom transfer redox process, i.e., R1R2S-->R1R2S=N-SO2R3, has been less reliable. In sulfilimine synthesis, sulfoxide has been an inevitable byproduct in all cases to date, and the yields of sulfilimine have varied widely. A nearly ideal procedure for the sulfide to sulfonyl sulfilimine transformation is described. Almost quantitative yields are achieved from a diverse set of sulfides and a broad range of the readily available sulfonyl nitrenoid sources known as chloramine salts (R3SO2NClNa), essentially by simply stirring them together in acetonitrile.  相似文献   

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A simple method is suggested for the preparation of 5-alkylsulfinyl-1-aryltetrazoles via oxidation of 5-alkylsulfanyltetrazoles with 34% peracetic acid in high yields under mild conditions.  相似文献   

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A simple procedure for the synthesis and further functionalization of 4,5-diaminopyrazoles using mild conditions is reported herein. The desired products were obtained in good yield, and the structures have been confirmed by X-ray crystallography.  相似文献   

7.
《Comptes Rendus Chimie》2015,18(7):752-757
We herein report on a novel, simple and straightforward method for the preparation of nickel bisdiphosphine hydrogen-evolving catalysts, so-called DuBois catalysts, from commercially available nickel hexaaqua salts. This method yields coordination complexes with the same physical characteristics as previously described for compounds prepared from the [Ni(CH3CN)6]2+ precursor. However, if hexaaquanickel(II) chloride is used as a precursor, a different nickel bisdiphosphine complex is formed, which incorporates chloride as an axial ligand. This complex displays a significantly different electrochemical behavior and a diminished activity for proton reduction as compared to classic DuBois catalysts.  相似文献   

8.
A simple and efficient methodology for the preparation of N-chlorinated hydantoins is presented. These versatile chlorenium sources were isolated in high yield after a simple recrystallization. Among the ten examples are the first chiral N-chlorohydantoins.  相似文献   

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Summary Sodium and potassium aluminium hydrides are readily obtained from aluminium chloride and sodium and potassium hydrides, respectively, using organoaluminium compounds as catalysts for the reaction.  相似文献   

10.
The preparation of high specific activity128I by neutron activation of KIO3 is described. The128I produced in a Szilard-Chalmers process is eluted with a water-isopropylamine mixture which dissolves only KI but not KIO3.  相似文献   

11.
A simple method is described for the preparation of activated carbon fibers (ACFs) coated with graphite nanofibers (GNFs). Low-pressure-plasma mixed-gas (Ar/O2) treatment of the ACFs led to the growth of GNFs on their surface. The growth was greater at higher power inputs, and from TEM observations the GNFs were seen to be of herringbone type. It was found that the N2 adsorption capacity of the ACFs did not sharply decrease, and that volume resistivity of the ACFs enhanced as a result of this treatment.  相似文献   

12.
《Tetrahedron letters》1988,29(39):4939-4942
A brief route for preparation of the L-hexenulose 4 from D-glucal 1 via furan intermediates 2 and 3 is described.  相似文献   

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The reaction of phosphites with derivatives of 5′-azido-uridine and 5′-azidoadenosine in the presence of nucleophiles is a simple method to obtain the corresponding 5′-amidophosphoric esters. The dependency of heterocyclic alkylation of reaction temperature and solver has been investigated.  相似文献   

18.
A simple, convenient and high-yielding one-pot method for the synthesis of 2-heterocycle-substituted imidazoles from the corresponding nitriles has been developed. The procedure is easily scaleable and the workup does not involve chromatography. This synthesis is also applicable to the preparation of imidazoles with electron-poor aryl substituents.  相似文献   

19.
Yeast lipase ( ) catalysed the reaction between ethyl (±)-2-chloropropionate and different aliphatic and aromatic amines yielding optically active amides.  相似文献   

20.
A new, simple method was reported to prepare PDMS membranes with micrometer size pores for microfluidic chip applications. The pores were formed by adding polystyrene and toluene into PDMS prepolymer solution prior to spin-coating and curing. The resulting PDMS membrane has a thickness of around 10 μm and macropores with a diameter ranging from 1 to 2 μm measured using scanning electron microscope (SEM) imaging. This PDMS membrane was validated by integrating it with PDMS microfluidic chips for protein separation using isoelectric focusing mechanism coupled with whole channel imaging detection (IEF-WCID). It has been shown that five standard pI markers and a mixture of two proteins, myoglobin and β-lactoglobulin, can be separated using these chips. The results indicated that this macroporous PDMS membrane can replace the dialysis membrane in PDMS chips for the IEF-WCID technique. The preparation method of macroporous PDMS membrane may be potentially applied in other fields of microfluidic chips.  相似文献   

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