- Distinct structures of inorganic-organic supramolecular assemblies based on discrete metallocyclic complexes incorporating flexible imidazole ligands: Syntheses, crystal structures and properties
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Three new interesting discrete dinuclear metallocyclic complexes, namely, {[Pd2(1)4](NO3)4· 2DMSO· 2H2O}n (4), [Pd2(2) 2Br4]n (5), and {[Pd2(3) 2Cl4]·4DMSO}n (6) have been successfully synthesized by the reaction of flexible exo-bidentate imidazole-containing ligands 1, 3-bis(imidazol-1-ylmethyl)benzene (1), 1, 3-bis(imidazol-1-ylmethyl)- 5-methylbenzene (2), and 2, 6-bis(imidazol-1-ylmethyl)-4-tert-butyl-phenol (3) with corresponding palladium salts. All these complexes were characterized by NMR spectroscopy in combination with elemental analysis, powder X-ray diffraction (PXRD), single-crystal X-ray diffraction, and thermal gravimetric analysis (TGA), respectively. Though all three complexes involve the similar supramolecular building blocks [2+2] metallocyclic units, under the inducement effect of the organic ligands, compounds 4-6 exhibit delicate geometric diversification of the resulting high-dimensional inorganic-organic supramolecular assemblies (e.g., [4+2] lantern-like cage structure, 1D channel, and 2D undulating framework, respectively). Furthermore, these results demonstrate that the secondary interactions such as intermolecular π ··· π stacking interactions and hydrogen bonds could play important roles in the aspect of linking low-dimensional entities into high-dimensional supramolecular frameworks.
- Yang, Li,Chang, Guanjun,Luo, Liang,Ding, Feng,You, Jingsong
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- Synthesis of two copper clusters and their catalysis towards the oxidation of benzene into phenol
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Reaction of a heptadentate ligand (H2LI) and a hexadentate ligand (H2LII) with three equivalents of Cu(ClO4)2·6H2O in methanol under basic conditions afforded a hexanuclear cluster [Cu6(LI)2(OH)4](ClO4)4·2DMF·3Et2O (1) and a nonanuclear cluster [(Cu9(LII)3(OH)7)](ClO4)5·0.25CH3OH·1.15H2O (2), respectively, where H2LI is 2,2′-(((pyridine-2,6-diylbis(methylene))bis((pyridin-2-ylmethyl)azanediyl))bis(methylene))diphenol and H2LII 2,2′-((((5-methyl-1,3-phenylene)bis(methylene))bis((pyridin-2-ylmethyl)azane-diyl))bis(methylene))bis(4-methylphenol). The structures of both clusters in their solid states have been determined by X-ray crystallography. Their magnetic susceptibilities reveal that both clusters are antiferromagnetic due to the coupling between the copper centers in the clusters. NMR spectroscopic analysis, conductivity measurements and ESI-MS analysis suggest that the clusters retain their structural integrities in solution. Both clusters show catalytic activity towards the hydroxylation of benzene into phenol with hydrogen peroxide (H2O2) as an oxidant at 80°C in aqueous acetonitrile. The conversion rate is about 20% and their TON/TOF are 564/188 and 905/302 for clusters 1 and 2, respectively.
- You, XiuLi,Wei, ZhenHong,Wang, HaiLong,Li, DongPing,Liu, Jian,Xu, BeiBei,Liu, Xiaoming
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p. 61790 - 61798
(2015/02/19)
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- Self-assembly from metal-organic vesicles to globular networks: Metallogel-mediated phenylation of indole with phenyl boronic acid
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Self-assembly of the conformationally flexible bismethylimidazolyl ligands with Pd(OAc)2 is described. Depending on whether the ligands provide the hydrogen bonding donor, a switching of metal-organic vesicles to globular networks gelating solvents is achieved. The metallogels exhibit catalytic activity for the cross-coupling of indole with phenyl boronic acid.
- Yang, Li,Luo, Liang,Zhang, Shuai,Su, Xiaoyu,Lan, Jingbo,Chen, Chi-Tien,You, Jingsong
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supporting information; scheme or table
p. 3938 - 3940
(2010/07/14)
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- Synthesis of 8-methyl[2.2]metacyclophanes and their charge-transfer complexes with tetracyanoethylene
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The regioselective 1:1 charge-transfer band of 13-substituted 8-methyl[2.2]metacyclophanes with tetracyanoethylene in CH2Cl 2, attributable to the 8-methyl substituted benzene-site complex, are observed in the field of 556-605 nm, which is strongly affected by π-electron density of the opposite aromatic ring.
- Shimizu, Tomoe,Hita, Katsuhiro,Rahman, Shofiur,Yamato, Takehiko
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experimental part
p. 293 - 297
(2009/12/07)
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- Process for the Preparation of 2,2'-[5-(1H-1,2,4-Triazole-1-Ylmethyl) -1,3-Phenylene] Di (2-Methylpropionitrile)
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The present invention discloses a process for the preparation of Anastrozole of the formula I in high purity and in high yield. 3,5-bis(halomethyl)toluene is prepared by reacting mesitylene with N-halosuccinimide in the presence of light or dibenzoyl peroxide or azobis isobutyronitrile as a catalyst and in a chlorinated solvent. 3,5-bis(halomethyl)toluene is cyanated with metal cyanide in the presence of a catalyst and in water, organic solvent or mixture thereof at temperature of 40 to 60° C. to obtain 2,2′-(5-methyl-1,3 phenylene)diacetonitrile which is further methylated with iodomethane in the presence of base and an organic solvent at temperature of 0 to 15° C. to obtain 2,2′-(5-methyl-1,3-phenylene)di(2-methyl-propiononitrile). The product obtained is treated with N-halosuccinimide in the presence of a catalyst and in a chlorinated solvent at temperature of 60 to 100° C. to obtain 2,2′-(5-halomethyl-1,3-phenylene)di(2-methyl propionitrile) which was further treated with potassium or sodium salt 1,2,4-triazole at temperature of 20 to 50° C. in dimethyl formamide to obtain crude 2,2′-[5-(1H-1,2,4-triazole-1-ylmethyl)-1,3-phenylene]di(2-methyl-propionitrile). The crude product is purified by column chromatography using a stationary phase and a mobile phase followed by recrystallization with a solvent or mixture of solvents to obtain highly pure Anastrozole.
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Page/Page column 5
(2008/12/08)
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- Affinity-based enrichment of phosphorylated peptides and/or proteins
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The invention relates to a substance comprising a solid carrier that is connected to a spacer by means of a linker, said spacer comprising at least two defined groups. Said substance is suitable for using as an affinity material for enriching and/or isolating phosphorylated peptides and/or proteins. The inventive substance especially enables tyrosine-phosphorylated peptides and/or proteins to be enriched and/or isolated.
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- Reversible photon-mode phosphorescence switching of heteroleptic cyclometalated iridium(III) complexes via photochromic bisthienylethene switch linked to ancillary ligand
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A novel class of heteroleptic IrIII complexes covalently linked with photochromic bisthienylethene (BTE) switch showed optically addressed modulation in blue, green, and yellow phosphorescence. Additional enhancement of phosphorescence modulati
- Lee, Insuk,You, Ngmin,Lim, Seon-Jeong,Park, Soo Young
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p. 888 - 889
(2008/02/12)
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- PROCESS FOR THE PREPARATION OF 2,2’-[5-(1,2,4-TRIAZOLE-1-YLMETHYL) -1,3-PHENYLENE] DI (2-METHYLPROPIONITRILE).
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The present invention discloses a process for the preparation of Anastrozole of the formula I in high purity and in high yield. 3,5-bis(halomethyl)toluene is prepared by reacting mesitylene with N-halosuccinimide in the presence of light or dibenzoyl peroxide or azobis isobutyronitrile as a catalyst and in a chlorinated solvent. 3,5-bis(halomethyl)toluene is cyanated with metal cyanide in the presence of a catalyst and in water, organic solvent or mixture thereof at temperature of 40 to 60° C to obtain 2,2'-(5-methyl-l,3 phenylene)diacetonitrile which is further methylated with iodomethane in the presence of base and an organic solvent at temperature of 0 to 15° C to obtain 2,2'-(5-methyl-l,3-phenylene)di(2-methyl-propiononitrile). The product obtained is treated with N-halosuccinimide in the presence of a catalyst and in a chorinated solvent at temperature of 60 to 100° C to obtain 2,2'-(5-halomethyl-l,3-phenylene)di(2-methyl propionitrile) which was further treated with potassium or sodium salt 1,2,4-triazole at temperature of 20 to 50° C in dimethyl formamide to obtain crude 2,2'-[5-(lH-l,2,4-triazole-l-ylmethyl)-l,3-phenylene]di(2- methylpropionitrile). The crude product is purified by column chromatography using a stationary phase and a mobile phase followed by recrystallization with a solvent or mixture of solvents to obtain highly pure Anastrozole.
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Page/Page column 13
(2008/06/13)
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- Process for the preparation of anastrozole and intermediates thereof
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A process for the preparation of anastrozole is provided, the process comprising: (a) reacting 3,5-bis(1-cyano-1-methylethyl)benzyl halide with a 4-Z-1,2,4-triazole compound of the formula wherein Z is a protecting group to produce 2,2′-[5-(4-Z-1,2,4-triazolium-1-ylmethyl)-1,3-phenylene]di(2-methylpropionitrile) halide; and (b) deprotecting the 2,2′-[5-(4-Z-1,2,4-triazolium-1-ylmethyl)-1,3-phenylene]di(2-methylpropionitrile)halide to produce anastrozole. Also provided is anastrozole substantially free of its isomers.
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Page/Page column 5-6
(2008/06/13)
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- Process for side-chain bromination of alkylbenzenes
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A process for the side-chain bromination of alkylbenzenes according to Formula (I) wherein R1 is C1-C6-alkyl; R2 is H or C1-C6-alkyl which can be unsubstituted or substituted by one or more cyano groups; R3 is H or C1-C6-alkyl which can be unsubstituted or substituted by one or more cyano groups; comprising the steps of (1) dissolving the compound of Formula (I) in a solvent which is a non-aromatic non-halogenated hydrocarbon which can be substituted by one or more cyano groups; (2) adding a bromination agent selected from the group consisting of Br2 and N-bromoimides to the solution; and optionally (3) agitating the mixture at a temperature within the range of from room temperature to reflux temperature.
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Page/Page column 3; 4
(2010/11/23)
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- Improved process for side-chain bromination of alkyl-benzenes
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A process for the side-chain bromination of alkylbenzenes according to Formula (I) wherein R1 is C1-C6-alkyl; R2 is H or C1-C6-alkyl which can be unsubstituted or substituted by one or more cyano groups; R3 is H or C1-C6-alkyl which can be unsubstituted or substituted by one or more cyano groups; comprising the steps of (1) dissolving the compound of Formula (I) in a solvent which is a nonaromatic non-halogenated hydrocarbon which can be substituted by one or more cyano groups; (2) adding a bromination agent selected from the group consisting of Br2 and N-bromoimides to the solution; and optionally (3) agitating the mixture at a temperature within the range of from room temperature to reflux temperature.
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- Complexes of Ag(i), Hg(i) and Hg(ii) with multidentate pyrazolyl-pyridine ligands: From mononuclear complexes to coordination polymers via helicates, a mesocate, a cage and a catenate
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The coordination chemistry of a series of di- and tri-nucleating ligands with Ag(i), Hg(i) and Hg(ii) has been investigated. Most of the ligands contain two or three N,N′-bidentate chelating pyrazolyl-pyridine units pendant from a central aromatic spacer;
- Argent, Stephen P.,Adams, Harry,Riis-Johannessen, Thomas,Jeffery, John C.,Harding, Lindsay P.,Clegg, William,Harrington, Ross W.,Ward, Michael D.
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p. 4996 - 5013
(2007/10/03)
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- Synthesis of monodeoxycalix[4]arene and its dimer structure in solution
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Monodeoxycalix[4]arene (3) has been synthesized by a stepwise condensation method. It forms dimer in solution, the structure of which has an arrangement of the two cone of 3 facing the respective narrower rim with each other. A cyclic hydrogen bonding array of six hydroxyl groups in the dimer was suggested from the thermodynamic parameters of the monomer-dimer equilibrium.
- Fukazawa,Deyama,Usui
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p. 5803 - 5806
(2007/10/02)
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