Poly(N-bromo-N-ethyl-benzene-1,3-disulfonamide), N,N,N′,N′-tetrabromobenzene-1,3-disulfonamide as new efficient reagents for conversion of alcohols to THP ethers and aldehydes to oxazoline compounds

This paper is concerned with an easy preparation of THP ethers from primary, secondary and tertiary alcohols and oxazoline compounds from various aldehydes using poly(N-bromo-N-ethyl-benzene-1,3-disulfonamide), N,N,N′,N′-tetrabromobenzene-1,3-disulfonamide [TBBDA] as new and efficient reagents under ambient conditions without over-oxidation.     

Poly(N,N′-dichloro-N-ethyl-benzene-1,3-disulfonamide, N,N,N′,N′-tetrachlorobenzene-1,3-disulfonamide, poly(N,N′-dibromo-N-ethyl-benzene-1,3-disulfonamide, and N,N,N′,N′-tetrabromobenzene-1,3-disulfonamide catalyzed formylation of amines and alcohols using ethyl formate under microwave irradiation

A simple, rapid, and efficient procedure for formylation of primary and secondary amines and alcohols using ethyl formate catalyzed with poly(N,N′-dichloro-N-ethyl-benzene-1,3-disulfonamide (PCBS), N,N,N′,N′-tetrachlorobenzene-1,3-disulfonamide (TCBDA), poly(N,N′-dibromo-N-ethyl-benzene-1,3-disulfonamide (PBBS) and also N,N,N′,N′-tetrabromobenzene-1,3-disulfonamide (TBBDA) was adopted. The reactions were performed under microwave irradiation with high yields.     

N,N,N′,N′-tetrabutylmalonamide as a new extractant for extraction of nitric acid and uranium(VI) in toluene

N,N,N,N-tetrabutylmalonamide (TBMA) was synthesized and used for extraction of uranyl(II) ion from nitric acid media in toluene. The effects of nitric acid concentration, extractant concentration, temperature and salting-out agent (LiNO₃) on distribution coefficients of uranyl(II) ion have been studied. The extraction of nitric acid is also studied. The main adduct of TBMA and HNO₃ is HNO₃. TBMA in 1.0 mol/l nitric acid solution. The 1:2:3 complex of uranyl(II) ion, nitrate ion and TBMA as extracted species is further confirmed by IR spectra of the extraction of uranyl(II) ion with TBMA, and found that the NO ₃ ^– in the extraction species UO₂(NO₃)₂·3TBMA did not participate in coordination of uranyl(II) ion. The values of thermodynamic parameters have also been calculated.     

N,N,N′,N′-tetrabutylsuccinylamide as a new extractant in n-dodecane for extraction of uranium(VI) and thorium(IV) ions

N,N,N,N-tetrabutylsuccinylamide (TBSA) was synthesized, characterised and used for the extraction of U(VI) and Th(IV) from nitric acid solutions into n-dodecane. Extraction distribution coefficients of U(VI) and Th(IV) as a function of aqueous nitric acid concentration, extractant concentration and temperature have been measured and found that n-dodecane as diluent was superior to 50% 1,2,4-trimethyl benzene (TMB) and 50% kerosene, (OK) system for extraction of U(VI) and Th(IV). The compositions of extracted species, equilibrium constants and enthalpies of extraction reactions have also been calculated. The formation of the 121 complex of uranyl(II) ion or the 141 complex of thorium(IV) ion, nitrate ion and TBSA and extracted species was further confirmed by the IR spectra of saturated extract of U(IV) and Th(IV).     

Metal derivatives of 1,3-bis(2-pyridyl)-1,3-propanedione and N,N′-dimethyl-1,3-bis(2-pyridyl)-1,3-propanedione

Complexes of transition metal ions with the oxygen-nitrogen containing ligand 1,3-bis(2-pyridyl)-1,3-propanedione (bpypH) have been synthesized. These present stoichiometries which do not conform with the usual tendency manifested by β-diketones, since molecular formulas with the composition M(bpyp)X are found. A nitrogen methylated ligand N,N′-dimethyl-1,3-bis(2-pyridyl)-1,3-propanedione methyl sulphate [dimebpypH] (MeSO₄)₂ has also been synthesized and its complexes with transition metal ions studied. The stoichiometries now, resemble those of typical β-diketones, namely [dimepyp]₂MX₄ with four anions because of the dicationic nature of the original ligand. This, together with IR evidence suggests a dual type of coordination by bpip via the β-diketone and the pyridyl moieties.     

Manganese(II), nickel(II) and copper(II) complexes of (1,3-bis-aminomethyl) cyclohexane-N,N,N′,N′-tetrakisbenzimidazole

Summary Mn^II, Ni^II and Cu^II complexes of (1,3-bis-aminomethyl)-cyclohexane-N,N,N,N-tetrakisbenzimidazole (CDTB) have been prepared and characterized by spectral techniques. The complexes are monomeric and pseudo-octa-hedral, as evidenced by their e.p.r. spectra and analytical data. Parameters ², ², ² and for Cu^II complexes, and the crystal field splitting parameter (10 Dq) together with the Nephelauxetic ratio (), for Ni^II complexes, are reported.     

Synthesis,acid-base and complexing properties of N,N,N′,N′-tetrakis(O-butylhydroxyphosphorylmethyl)-1,2-diaminoethane

Russian Journal of General Chemistry - A method of synthesis of organophosphorus analog of ethylenediaminetetraacetic acid (a common complexon),...     

Synthesis and characterization of N,N,N′,N′-tetraalkyl-4-oxaheptanediamide as extractant for extraction of uranium(VI) and thorium(IV) ions from nitric acid solution

Tridentate ligand N,N,N′,N′-tetraoctyl-4-oxaheptanediamide(TOOHA) and other three analogous diamides have been prepared and characterized by using NMR spectra and element analysis. The extraction of UO₂ ²⁺ and Th⁴⁺ with the present extractants was investigated at 293 ± 1 K from nitric acid solutions. n-Octane was found to be the most suitable diluent in the present study compared with other diluents tested. Extraction distribution ratios (D) of U(VI) and Th(IV) have been studied as a function of aqueous concentrations of HNO₃, extractant concentrations. The results indicated that U(VI) is mainly extracted as UO₂(NO₃)₂·2TOOHA. In the case of Th⁴⁺ ion, the possible compositions of extracted species in organic phase were presumed to be Th(NO₃)₄·2TOOHA and Th(NO₃)₄·3TOOHA. In addition, the influence of concentration of sodium nitrate as salting-out agent on the distribution ratio of U(VI) and Th(IV) with TOOHA was also evaluated.     

Five coordinate complexes of N,N,N′,N′-tetraethylpyridine-2,6-dicarboxamide with copper Crystal and molecular structures of dichloro(N,N,N′,N′-tetraethylpyridine-2,6-dicarboxamido)copper(II) and chloro(perchlorato)(N,N,N′,N′-tetraethylpyridine-2,6-dicarboxamido)copper(II)

The title compound N,N,N′,N′-tetraethylpyridine-2,6-dicarboxamide (DEAP) forms a 1:1 complex with anhydrous CuCl₂, [Cu(DEAP)Cl₂], (1) which was crystallized from EtOH solution in the monoclinic space group P2_{1/ n} with cell constant, a = 10.024(1); b = 13.122(1); c = 14.404(1) Å β = 101.31(1)° V = 1857.8(3) ų and Z = 4. The chloro-perchlorato complex, [Cu(DEAP)Cl(ClO₄)], (2) obtained in near quantitative yield by reacting (1) with an excess of NaClO₄ in EtOH, crystallized in the monoclinic space group P2_{1/ n} with cell constants, a = 7.965(1); b = 25.827(2); c = 10.046(1) Å β = 98.81(1)° V = 2042.2(4) ų and Z = 4. Both (1) and (2) contain 5-coordinated copper linked to DEAP through O～N～O donor set of atoms with covalently bonded chlorine atoms in (1) and chlorine and perchlorate groups in (2). The coordination geometry is intermediate between square pyramidal and trigonal bipyramidal, and is probably best described as a trigonally distorted rectangular pyramid.     

Cyclic seleninate esters as catalysts for the oxidation of sulfides to sulfoxides, epoxidation of alkenes, and conversion of enamines to α-hydroxyketones

Cyclic seleninate esters serve as catalysts for the rapid oxidation of sulfides to sulfoxides, alkenes to epoxides, and enamines to α-hydroxyketones. Optimal conditions were found that minimize the overoxidation of the product sulfoxides to sulfones and the hydrolysis of epoxides to diols. In some examples such as styrene derivatives, oxidative cleavage was observed instead of epoxidation. The enamine oxidations proceed via the initial formation of dimeric 2,5-diamino-1,4-dioxane species, which were hydrolyzed in situ to the final products. The structure of one such dimer was confirmed by X-ray crystallography.     

Synthesis,characterization and application of nano-N,N,N′,N′-tetramethyl-N-(silica-n-propyl)-N′-sulfo-ethane-1,2-diaminium chloride as a highly efficient catalyst for the preparation of N,N′-alkylidene bisamides

Research on Chemical Intermediates - A novel mesoporous nanomaterial, namely nano-N,N,N′,N′-tetramethyl-N-(silica-n-propyl)-N′-sulfo-ethane-1,2-diaminium chloride...     

Synthesis,Crystal Structure and Spectroscopic Properties of N,N′-Diphenyl-N,N′-bis(2-fluorophenyl)-1,1′-biphenyl-4,4′-diamine

A fluorinated tetraphenylbenzidine derivative, N,N′-diphenyl-N,N′-bis(2-fluorophenyl)-1,1′-biphenyl-4,4′-diamine (C36H26F2N2, Mr = 524.59) was synthesized via the palladiumcatalyzed Buchwald-Hartwig reaction of N,N′-diphenyl-1,1′-biphenyl-4,4′-diamine with 2-fluoroiodobenzene (yield: 75%) and structurally characterized. It crystallizes in monoclinic, space group P21/n with a = 9.820(7), b = 14.305(11), c = 10.233(8) , β = 108.973(9)o, V = 1359.3(18) 3, Z = 2, Dc = 1.282 g/cm3, μ(MoKα) = 0.084 mm-1, F(000) = 548, S = 1.018, the final R = 0.0439 and wR = 0.0928. It presents a linear centrosymmetric framework constituted by a linkage of biphenyl as a bridge and two fluorinated diphenylamine moieties. The UV-Vis absorption and fluorescence spectra of the title compound were also investigated. This compound emits intense blue fluorescence with a peak wavelength of 406 nm in film.     

KBrO3/MoO3： An efficient reagent system for the oxidative deprotection of semicarbazones, 1,1-diacetates and acetals

Semicarbazones,1,1-diacetates and acetals are efficiently converted to their corresponding carbonyl compounds using synergistic effect between KBrO3 and MoO3 in refluxing CH3CN-H20 in good to high yields.     

N′N′N pincer and N′N bidentate(pyrazolylpyridyl) Rh(I) complexes as catalyst precursors for hydroformylation of olefins

Transition Metal Chemistry - The industrial process of hydroformylation or the oxo process has been used for many years in the production of aldehydes from alkenes. Different metals have been used...     

Synthesis of Bisindolylindeno[1,2-b]quinoxaline and Bisindolylindeno[3,4-b]pyrazine with Poly(N,N′-dibromo-N-ethylnaphthyl-2,7-disulfonamide)

Poly(N,N′-dibromo-N-ethylnaphthyl-2,7-disulfonamide) (PBNS) as novel reagent was synthesized. Bisindolylindeno[1,2-b]quinoxaline and bisindolylindeno[3,4-b]pyrazine derivatives were synthesized in a simple and efficient method from the three-component condensation reaction of indole, indane-1,2,3-trione, and diamine aromatic compounds by PBNS under solvent-free conditions at 80 °C in good to excellent yields, short reaction times, and a simple procedure for new derivatives.

[Supplementary materials are available for this article. Go to the publisher's online edition of Synthetic Communications^® for the following free supplemental resource(s): Full experimental and spectral details.]     

Transient Absorption Spectral Characterization of Electron Transfer between Fullerenes (C_(60)/C_(70)) and N,N,N′,N′-Tetra(p-methylphenyl)-4,4′-diamino-1,1′-diphenyl Sulphide (TPDAS)

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