Tf2O as a CF3 Source for the Synthesis of Trifluoromethoxylation Reagent nC4F9SO3CF3.

Described herein is the convenient synthesis of an efficient trifluoromethoxylation reagent, nC4F9SO3CF3, by using cheap and widely available reagents and without the need of any tedious column chromatography purification procedure.

Diaqua-bis-[4-(1H-imidazol-2-yl)pyridine-κN]bis-(nitrato-κO)cadmium.

In the title compound, [Cd(NO3)2(C8H7N3)2(H2O)2], the Cd(II) cation is situated on an inversion center and is coordinated by the O atoms of two nitrate anions, by the N atoms of two 4-(imidazol-2-yl)pyridine ligands and by two water O atoms in a slightly distorted N2O4 octa-hedral geometry. The dihedral angle between the imidazole and pyridine rings is 1.6 (2)°. In the crystal, mol-ecules are linked by N-H⋯O, O-H⋯N and O-H⋯O hydrogen bonds, forming a three-dimensional network.

catena-Poly[[silver(I)-µ-bis-{2-[(E)-phenyl-diazen-yl]-1H-imidazol-1-yl}methane] trifluoro-methane-sulfonate].

The title compound, {[Ag(C(19)H(16)N(8))](CF(3)SO(3))}(n), is a coordin-ation polymer with cationic chain motif. The Ag(+) cation is coordinated by two unsubstituted imidazolyl N atoms of two independent 2-paBIM ligands [2-paBIM is bis-{2-[(E)-phenyl-diazen-yl]-1H-imidazol-1-yl}methane]. The shortest Ag⋯Ag separation in a cationic chain is 8.841 (2) Šand the dihedral angle between two 2-phenyl-diazenyl-imidazole planes in the same ligand is 74.7 (3)°. Weak C-H⋯O interactions are seen in the crystal.

Difluorocarbene-based cyanodifluoromethylation of alkenes induced by a dual-functional Cu-catalyst.

Although cyanofluoroalkylation has received increasing attention, a toxic cyanation reagent is usually required. Herein, a Cu-catalyzed difluorocarbene-based cyanodifluoromethylation of alkenes with BrCF2CO2Et/NH4HCO3 under photocatalytic conditions is described. BrCF2CO2Et and NH4HCO3 serve as a carbon source and a nitrogen source of the nitrile group, respectively, avoiding the use of a stoichiometric toxic cyanation reagent. The Cu-complex plays a dual role. It is not only a photocatalyst, but also a coupling catalyst for the formation of a C-CN bond.

1-[(Phenyl-iminio)amino]-2-naphtho-late.

In the zwitterionic title compound, C(16)H(12)N(2)O, the dihedral angle between the benzene ring and naphthalene ring system is 2.0 (1)°. The azo group adopts a trans configuration and an intra-molecular N-H⋯O hydrogen bond is found. In the crystal, the mol-ecules are packed by strong π-π inter-actions [centroid-centroid distance between aromatic rings = 3.375 (3) Å].

Calix[4]arene crown-4 ether modified glassy carbon electrode for electrochemical determination of norepinephrine.

A sensitive and selective electrochemical method for the determination of norepinephrine (NE) was developed by using a calix[4]arene crown-4 ether (CACE) film modified glassy carbon electrode (GCE). The fabrication of the CACE film and its electrocatalytic effect for electrochemical oxidation of NE were investigated by electrochemical impedance spectroscopy (EIS) and voltammetric methods. It was found that the electrochemical behavior of NE on the CACE film modified electrode depended on the film thickness of CACE. Based on the electrochemical data, the CACE film surface coverage (theta), the charge transfer number (z) and the amount of the surface-bound NE (Gamma) were calculated. The effects of the experimental variables such as the solution pH and the applied potential were investigated for optimum analytical performance. Excellent linear relationships were obtained in two concentration ranges of NE: one was from 0.55 to 9.7 microM and the other was 9.7 to 230 microM. The detection limit (S/N = 3) of NE obtained by steady-state amperometry was 0.28 microM. The relative standard deviation (RSD) for 10 successive measurements of 0.05 mM NE was 2.2%. This method could be applied for the direct determination of NE in injection samples. In addition, effects of possible interferences (e.g. ascorbic acid, AA) were investigated. The present work provides an effective method for amperometric determination of NE by using a CACE modified electrode.

3-Benzyl-1-methyl-imidazolium picrate.

In the title salt, C(11)H(13)N(2) (+)·C(6)H(2)N(3)O(7) (-), the dihedral angles between the benzene ring in the cation and the imidazolium ring and the benzene ring of the picrate anion are 113.7 (2) and 116.3 (2)°, respectively. The imidazolium ring is nearly parallel to the benzene ring of the picrate anion, the dihedral angle between the planes being 2.6 (1)°. The nitro groups in the picrate anions are disordered (occupancy ratio 0.54:0.46). The crystal packing is stabilized by weak C-H⋯O inter-actions between the cation-anion pairs.

3,3'-Dibenzyl-2,2'-dimethyl-1,1'-methyl-enediimidazolium dipicrate.

In the title salt, C(23)H(26)N(4) (2+)·2C(6)H(2)N(3)O(7) (-), the dihedral angle between the imidazolium rings in the dication is 69.9 (1)°. The aromatic ring of the benzyl group is almost perpendicular to the N-heterocyclic ring that is directly connected to it [dihedral angles = 83.2 (2) and 77.3 (3)°].

1-(4-Methyl-phenyl-diazo-nium-yl)-2-naphtholate.

In the title compound, C(17)H(14)N(2)O, the dihedral angle between the benzene ring and naphthalene ring system is 11.0 (3)°. The azo group adopts an anti configuration and an intra-molecular N-H⋯O hydrogen bond exists. Mol-ecules are packed by π-π inter-actions between adjacent mol-ecule (closest approach between centroids of benzene and naphthalene rings of 3.501 Å).

A new infinite inorganic [n]catenane from silver and bis(2-methylimidazolyl)methane ligand.

A new type of 1D infinite inorganic [n]catenane framework was self-assembled by silver nitrate and bis(2-methylimidazolyl)methane, while a comparatively one-dimensional zigzag cationic chain was generated by AgNO(3) and bis(imidazol-1-yl)methane.

Catena-poly[[dinitratocadmium(II)]bis[mu-bis(2-methyl-1H-imidazol-1-yl)methane-kappa(2)N(3):N(3')]].

The title compound, [Cd(NO(3))(2)(C(9)H(12)N(4))(2)](n), has a one-dimensional double-bridged chain polymer structure with a 16-membered macrometallacyclic tetragonal structural motif. The Cd(II) ion occupies a crystallographic inversion centre and is coordinated by four equatorial N atoms from four distinct bis(2-methylimidazol-1-yl)methane ligands and two apical nitrate O atoms to form a slightly distorted octahedral coordination geometry.

Syntheses and characterization of unsymmetric dicationic salts incorporating imidazolium and triazolium functionalities.

A series of both imidazolium- and triazolium-based unsymmetric dicationic salts with alkyl and polyfluoroalkyl substituents were prepared and characterized. Most of them can be classified as ionic liquids (MP < 100 degrees C). Key physical properties, such as melting point, thermal stability, density, and solubility in common solvents were determined and were compared with those of the related monocationic imidazolium- or triazolium-based salts. The effects of anions and substituents bonded to the triazolium and imidazolium cations on these properties were examined. 1-(3-Butyl-imidazolium-1-yl)methylene-(4-butyl-1,2,4-triazolium diiodide) (2d), the precursor of 1-(3-butylimidazolium-1-yl)methylene-(4-butyl-1,2,4-triazolium) bi[bis(trifluoromethanesulfonyl)amide] (3d), reacted with Pd(OAc)(2) at 120 degrees C to generate a binuclear palladium(II) dicarbene complex. The palladium(II) complex was characterized by single-crystal X-ray diffraction analysis and was used as a catalyst precursor for palladium-catalyzed Heck cross-coupling reactions in 3d. Preliminary results show that 3d could serve as both the solvent and catalyst support in the catalytic reactions.

Bridged di(alkyl- and 4,4,4-trifluorobutylimidazolium) quaternary salts based on p-tert-butylcalix[4]arene.

Di(alkyl- and 4,4,4-trifluorobutylimidazolium) quaternary halides of p-tert-butylcalix[4]arene, 5a-8a and 11a, were prepared and characterized. Metathetical reactions of these compounds with LiN(SO(2)CF(3))(2) and KPF(6) in methanol and water gave the corresponding new quaternary salts 5b-8b and 11b and 5c-8c and 11c, respectively, with high thermal stabilities. Compounds 5a-d, 6b, and 11a-c exhibit melting points <100 degrees C. On the basis of (1)H NMR and (13)C NMR spectral measurements, all of the new quaternary calix[4]arene salts were found to exist in a cone conformation. (1)H NMR titration experiments and electrospray MS spectra support the encapsulation of K(+) in the ionophoric cavity of 11c.