Facile synthesis of 2-azaazulenes from thiobenzoyl isocyanates using trimethylsilyldiazomethane

The reaction of trimethylsilyldiazomethane with thiobenzoyl isocyanates, in situ generated from thiazole-4,5-diones, yielded diazoketones, which were converted into 2-azaazulenes by the intramolecular Buchner reaction.     

Perturbation method for determining the group of invariance of hierarchical models

We propose a perturbation method for determining the (largest) group of invariance of a toric ideal defined in [S. Aoki, A. Takemura, The largest group of invariance for Markov bases and toric ideals, J. Symbolic Comput. 43 (5) (2008) 342–358]. In the perturbation method, we investigate how a generic element in the row space of the configuration defining a toric ideal is mapped by a permutation of the indeterminates. Compared to the proof by Aoki and Takemura which was based on stabilizers of a subset of indeterminates, the perturbation method gives a much simpler proof of the group of invariance. In particular, we determine the group of invariance for a general hierarchical model of contingency tables in statistics, under the assumption that the numbers of the levels of the factors are generic. We prove that it is a wreath product indexed by a poset related to the intersection poset of the maximal interaction effects of the model.     

Refractive index detection in microbore column liquid chromatography

Summary An existing commercial refractive index detector was modified for use with microbore column LC systems. The detector utilizes the Fresnel method. The effect of band dispersion and dilution at the detector side is of extreme importance in connection with the miniaturized LC system. In the modified model the original heat-exchanger tube was removed and a stainless steel capillary was used for heat-exchanging. Gaskets having different cell volumes were also examined with respect to band broadening and sensitivity. The detection limit was 10ng for di-n-pentyl phthalate. The examples include the detection of phthalates, alcohols, n-paraffins, and kerosine.     

Refractive index detection in slurry-packed capillary column LC

An existing commercial refractive index detector was modified for use with slurry-packed capillary column LC systems. The cell gasket of the original detector cell was replaced by a micro cell gasket giving a volume of 0.8 μL. The relationship between detector response and the amount of sample injected was examined. The limit of detection was 2-3 ng for di-n-pentyl phthalate.     

A noncontact atomic force microscope in air using a quartz resonator and the FM detection method

Noncontact imaging was successfully performed with the quartz resonator in air by using the FM detection method. A constant frequency shift mode was used. The frequency shift was about -30 mHz, which was induced by the attractive force gradient. A noncontact image of the Si(111) atomic step was obtained with vertical and lateral resolutions of 0.8 Å and 60 Å.     

Empirical characteristic function approach to goodness-of-fit tests for the Cauchy distribution with parameters estimated by MLE or EISE

We consider goodness-of-fit tests of the Cauchy distribution based on weighted integrals of the squared distance between the empirical characteristic function of the standardized data and the characteristic function of the standard Cauchy distribution. For standardization of data Gürtler and Henze (2000,Annals of the Institute of Statistical Mathematics,52, 267–286) used the median and the interquartile range. In this paper we use the maximum likelihood estimator (MLE) and an equivariant integrated squared error estimator (EISE), which minimizes the weighted integral. We derive an explicit form of the asymptotic covariance function of the characteristic function process with parameters estimated by the MLE or the EISE. The eigenvalues of the covariance function are numerically evaluated and the asymptotic distributions of the test statistics are obtained by the residue theorem. A simulation study shows that the proposed tests compare well to tests proposed by Gürtler and Henze and more traditional tests based on the empirical distribution function.     

Studies on proton pump inhibitors. I. Synthesis of 8-[(2-benzimidazolyl)sulfinyl]-5,6,7,8-tetrahydroquinolines and related compounds

Many 8-[(2-benzimidazolyl)sulfinyl]-5,6,7,8-tetrahydroquinolines were synthesized and examined for their (H+ + K+) adenosine triphosphatase ATPase-inhibitory and antisecretory activities. These sulfinyl compounds could be considered to be rigid analogues of the 2-[(2-pyridyl)methylsulfinyl]benzimidazole class of antisecretory agents. All the compounds tested were potent inhibitors of (H+ + K+)ATPase. Most of the compounds also inhibited histamine-induced gastric acid secretion in rats. Among them, 8-[(5-fluoro-2-benzimidazolyl)sulfinyl]-3-methyl-5,6,7,8-tetrahydroqu inoline (XIVm) was found to have the most potent activity. The structure-activity relationships are discussed.     

An 8-sulfonamidoquinoline derivative with imidazolium unit as an extraction reagent for use in ionic liquid chelate extraction systems

To evaluate the superiority of using a task-specific onium salt (TSOS), a novel TSOS reagent 1-methyl-3-[2-(8-quinolinylaminosulfonyl)ethyl]imidazolium chloride (HmimesqCl) was synthesized, and its performance in extraction of different divalent metal cations was investigated. This TSOS reagent has both a cationic imidazolium unit and an anionic (proton-dissociable) complexation unit for the extraction of metal cations into an ionic liquid. In the use of HmimesqCl, relatively high extraction of metals resulted in comparison with the use of its non-imidazolium analogs, without changing the extraction selectivity.