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11.
A family of homochiral metal carboxylate coordination polymers have been synthesized by treating 2,2'-dihydroxy-1,1'-binaphthalene-6,6'-dicarboxylic acid (H(2)BDA) with metal salts at elevated temperatures. BDA ligands link adjacent metal centers to form 1D coordination polymeric chains using the carboxylate functionality, while the hydroxyl groups of BDA ligands form H-bonds with carboxylate oxygen atoms to link 1D coordination polymeric chains into open frameworks of higher dimensionality. We also present evidence for the important role played by H-bonds in the stabilization of open framework structures which allows for the hierarchical assembly of chiral porous solids. 相似文献
12.
Eric Steiner Carl Djerassi Ernesto Fattorusso Silvana Magno Luciano Mayol Circo Santacroce Donato Sica 《Helvetica chimica acta》1977,60(2):475-481
Two acetylenic steroids, cholest-5-en-23-yn-3β-ol ( 5 ) and 26,27-dinorcholest-5-en-23-yn-3β-ol ( 3 ), and another unsaturated steroidalcohol, stigmasta-5,23-dien-3β-ol ( 7 ), were isolated from the sponge Calyx nicaaensis. The structures of these two acetylenic steroids were established by synthesis. Several attempts to synthesize the marine steroids alcohol calysterol ( 1 ), with a cyclopropene-containing side chain, starting from cholest-5-en-23-yn-3β-ol are also recorded. Addition of ethyl-diazo-acetate to the triple bond was performed, but the reduction to the methyl derivative yielded decomposition products. 相似文献
13.
A rapid and sensitive flow-injection method is described for the fluorimetric determination of the proteolytic activity of a number of enzymes. The substrate, fluorescein-labelled bovine serum albumin coupled to a 2-fluoro 1-methylpyridinium salt-activated Fractogel support, is packed in a small reactor (35 × 2 mm i.d.) and inserted into a flow manifold. Under the reaction conditions the amount of fluorescein released from enzymatic cleavage of the substrate is found to be directly proportional to the activity of the proteolytic enzyme. Sample throughput is 30–35 h?1. The calibration range for trypsin is linear up to at least 0.35 μg ml?1. Linear responses were also obtained for otherproteolytic enzymes such as papain, chymotrypsin, ficin and bromelain. 相似文献
14.
James D. Korp Ivan Bernal Nikolaus H. Fischer Charles Leonard Ihl-Young Lee Ngo LeVan 《Journal of heterocyclic chemistry》1982,19(1):181-187
The isolation and structure determination of two new guaianolides, pumilin and its 2,3-epoxide, from Berlandiera pumila and B. texana are reported. The structure of pumilin was determined from nmr and mass spectral data, and from an X-ray single crystal study; the structure of the epoxide was found by comparison of nmr spectra. Pumilin is shown to be a Δ1(10)-cis-guaianolide with a cyclopentenone ring attached to C1 and C5, and an α-methylene-γ-lactone ring trans-fused to C6 and C7. The absolute configuration was inferred from spectral considerations and knowledge of previous structural determinations. The cd spectrum of pumilin exhibits a negative Cotton effect, and the lactone chromophore has left-handed chirality. The cyclo-heptene ring is in the chair configuration, with the lactone a half-chair and the cyclopentenone essentially planar. Crystals are orthorhombic, a = 7.065, b = 13.652, c = 19.586 Å, space group P212121, Z = 4, and the final R value is 3.9%. The crystal structure is strengthened by an O···O hydrogen bond linking the molecules into infinite chains. 相似文献
15.
Bronger RP Silva SM Kamer PC van Leeuwen PW 《Dalton transactions (Cambridge, England : 2003)》2004,(10):1590-1596
A highly active and regioselective catalyst obtained from a novel dicationic ligand (1) and Rh(CO)2(acac) for hydroformylation of 1-hexene and 1-octene in ionic liquids is reported. Optimisation studies of various reaction parameters led to an unprecedentedly active (TOFs > 6200 mol mol(-1) h(-1), T= 100 degrees C), selective (l/b ratios > 40) and stable hydroformylation procedure. No catalyst leaching (Rh-loss < 0.07% of initial rhodium intake, P-loss < 0.4% of the initial phosphorus intake) or losses in performance could be measured during 1-octene hydroformylation recycle experiments in 1-butyl-3-methylimidazolium hexafluorophosphate. At low catalyst loadings activities and regioselectivities competitive with one-phase catalysis in conventional solvents were observed. At high catalyst loadings the system is extremely stable and has a long shelf-life as a result of the formation of stable, if inactive rhodium dimers. 相似文献
16.
Biosensors designed for environmental and food quality control based on screen-printed graphite electrodes with different configurations 总被引:3,自引:0,他引:3
Avramescu A Andreescu S Noguer T Bala C Andreescu D Marty JL 《Analytical and bioanalytical chemistry》2002,374(1):25-32
Graphite electrodes fabricated by screen-printing have been used as amperometric detectors in biosensors based on NAD(+)-dependent dehydrogenases, tyrosinase, or genetically modified acetylcholinesterases. The mono-enzyme sensors have been optimized as disposable or reusable devices for detection of a variety of substrates important in the food industry ( D-lactic acid, L-lactic acid, acetaldehyde) or in environmental pollution control (phenols and dithiocarbamate, carbamate and organophosphorus pesticides). The sensors were prepared in four configurations differing in enzyme confinement, enzyme immobilization and location of the immobilization agent in the biosensor assembly. Tests on real samples have been performed with the biosensors; D-lactic acid and acetaldehyde have been detected in wine and phenols in air. 相似文献
17.
The photolysis of a benzene solution of [Tp(Me2)IrH(2)(COE)], 1 (Tp(Me2) = hydrotris(3,5-dimethylpyrazolyl)borate, COE = Z-cyclooctene), in the presence of P(OMe)(3), gives the stable novel complex [Tp(Me2)IrH(C(6)H(5))(P(OMe)(3))], 3a. The photochemical syntheses of [Tp(Me2)IrH(2)(P(OMe)(3))], from 1 and P(OMe)(3) in diethyl ether, and [Tp(Me2)IrH(2)(CH(2)=CHCOO(t)Bu)], from 1 in tert-butyl acrylate, are also reported. The above reactions and several experiments using C(6)D(6) and P(OCD(3))(3) show that, in all cases, the primary photoproduct is the 16-electron, five-coordinate iridium(III) intermediate {Tp(Me2)IrH(2)}, 6a, produced by loss of COE from 1. The above experiments also allow the postulation of a mechanistic pathway for the formation of 3a which involves the oxidative addition of an aromatic C-H bond by 6a. Furthemore, the photochemical reaction of 1 in the presence of P(OCD(3))(3) shows that, under the reaction conditions used, oxidative addition of C-H bonds of P(OMe)(3) and of coordinated Tp(Me2)-ligands, presumably, to the intermediates 6a and {Tp(Me2)IrH(C(6)H(5))}, also occurs. Thus, coordinatively unsaturated iridium(III) species readily activate C-H bonds. 相似文献
18.
Slobodanka Stankovi Duan Lazar Ljubica Medi‐Mija
evi Katarina Penov‐Gai Marija Saka
Silvana Andri Bruvo Milenko 《Acta Crystallographica. Section C, Structural Chemistry》2002,58(3):o172-o173
The title molecule, C26H30O3, shows a novel chemical rearrangement of the substituents at position 17, i.e. an α‐orientation of the hydroxy group and a β‐orientation of the bulky benzyl moiety. The packing arrangement consists of coils formed by O2?O3 hydrogen bonds along the c axis. The compound shows complete loss of oestrogenic activity, and neither does it exhibit an antagonistic effect. 相似文献
19.
Luigia Serpico Mauro De Nisco Flavio Cermola Michele Manfra Silvana Pedatella 《Molecules (Basel, Switzerland)》2021,26(9)
A simple and efficient route for the synthesis of new glycoconjugates has been developed. The approach acts as a model for a mini-library of compounds with a deoxy-selenosugar core joined to a polyphenolic moiety with well-known antioxidant properties. An unexpected stereocontrol detected in the Mitsunobu key reaction led to the most attractive product showing a natural d-configuration. Thus, we were able to obtain the target molecules from the commercially available d-ribose via a shorter and convenient sequence of reactions. 相似文献
20.
Castellano PM Vignaduzzo SE Maggio RM Kaufman TS 《Analytical and bioanalytical chemistry》2005,382(7):1711-1714
A new, repeatable, and rapid method has been developed for resolution of binary mixtures of acetaminophen and diclofenac with minimum sample pretreatment and without separation of the analytes. The method, based on the PLS1 processing of absorbance data in the UV region, was successfully used for quantification of the drug content of three tablet preparations. The results obtained were in good agreement with HPLC recovery data. The method also enabled determination of drug-dissolution profiles of these commercial tablets, by simultaneous determination of both analytes during the dissolution test. 相似文献