Studies on the syntheses of heterocyclic compounds. Part CDXCVII. Total syntheses of (±)-cryptaustoline and (±)-thaliporphine by the benzyne reaction

The indisputable benzyne reaction of 1-(5-bromo-3,4-dimethoxybenzyl)-1,2,3,4-tetrahydro-7-hydroxy-6-metlioxy-2-methylisoquinoline (II) with sodium amide in liquid ammonia afforded the following compounds, (±)-cryptaustoline iodide (VI), (±)-thaliporphine (VIII), 1 -(3,4-dimeth-oxybenzyl)- (III), and 1 -(2-amino-4,5-dimethoxybenzyl)-l,2,3,4-tetrahydro-7-hydroxy-6-meth-oxy-2-methylisoquinoline (IV).     

Photocatalytic intercalated material based on HLaNb_2O_7 as host and Cd_(0.8)Zn_(0.2)S as guest

A novel photocatalytic material (Pt,Cd0.8Zn0.2S)/HLaNb2O7 was fabricated by successive intercalation and exchange reactions. The (Pt,Cd0.8Zn0.2S)/HLaNb2O7 possessed a gallery height less than 0.5 nm and showed a broad absorption with wavelength over 370―500 nm. Using (Pt,Cd0.8Zn0.2S)/HLaNb2O7 as catalyst, the photocatalytic H2 evolution was more than 160 cm3·h-1·g-1 in the presence of Na2S as a sacrificial agent under irradiation with wavelength more than 290 nm from a 100-W mercury lamp. Furthermore, the catalyst showed photocatalytic activity even under visible light irradiation.     

Studies on the syntheses of heterocyclic compounds. Part CCCXV erythrinan and related compounds. II . An alternative synthesis of cis-16-hydroxy-15-methoxyerythrinan-8-one and its mass spectrum

Phenolic cyclization of 2-ethoxycarbonylmethylidenecyclohexanone (IV) with 3-hydroxy-4-methoxyphenethylamine (V) were performed in the process of finding a synthetic approach to dihydroerysolidine (I). Thus, 16-hydroxy-15-methoxyerythrinan-6-ene-8-one (VI) and 16-hydroxy-15-methoxyerythrinan-7-ene-8-one (VII) were synthesized, both of which were hydrogenated in the presence of Adams platinum to give the same product (XI). Furthermore, on the basis of the mass spectra of XI and XII, these compounds were assumed to be stereoisomeric at the C₅- and C₆-positions.     

Luminescent palladium complexes containing thioamide-based SCS pincer ligands

Thioamide-based tridentate ligands, 1,3-benzenedicarbothioamides (1a-c), were used to afford pincer palladium(II) complexes (Pd(1-H)Cl, 2a-c) with η³-S,C,S type coordination. The complexes exhibit strong emission in a glassy frozen state as well as in the solid state. The decay lifetime of the emission from the complexes is in a range of 8-9 × 10⁻⁵ s, which is indicative of phosphorescent emission.     

Photolysis of vinyl bromides in the presence of tetrabutylammonium azide: trapping of a vinyl cation with azide ion

Vinyl cations generated by the title photolysis gave vinyl azides by capture of an azide ion and their further photolyses resulted in the formation of cycloaddition-products via nitrile ylides derived from the corresponding azirines.     

A study on the utilization of the Youden plot to evaluate proficiency test results

Methods of utilizing the Youden plot obtained from interlaboratory comparison tests are proposed. The Youden plot is a powerful tool for visually evaluating between- or within-laboratory errors. However, there are no generally applicable methods to indicate the anomalies in the between- and the within-laboratory errors in qualitative terms. An evaluation frame was therefore developed in this study as an indication method. Moreover, the Youden plot is considered to be useful for visually assessing the comprehensive performance of laboratories using two types of results. Although the confidence ellipse has been proposed in ISO 13528:2005 for this purpose, robust determination of the parameters has not yet been implemented. In the present study, robust determination of one of the parameters, the correlation coefficient, was developed. Our proposals were analytically validated using two types of statistical models. In addition, the properties were evaluated through computational simulations. From the results obtained, it can be concluded that our proposals are practically applicable to actual interlaboratory comparison tests.     

Measurement of the magnetic field of resin-impregnated bulk superconductor annuli

Large single-grain bulk RE–Ba–Cu–O (RE: rare earth elements) superconductors can trap large fields exceeding several teslas and thus can function as very strong quasi-permanent magnets. We have found that the resin can penetrate into a bulk superconductor, when the sample was immersed in molten resin. Hence, resin impregnation was effective in improving mechanical properties. Three bulk superconductors‘ annuli with resin impregnation, each 50-mm i.d. and 80-mm o.d. was built and energized, by a field-cool method, to generate, in a bath of liquid nitrogen, a persistent trapped field of 1.62 T.     

Preparation and photocatalytic activity of visible light-active sulfur and nitrogen co-doped SrTiO3

Nitrogen and sulfur co-doped SrTiO₃ was prepared by high energy grinding of the mixture of SrTiO₃ and thiourea. A new band gap in visible light region (522 nm) corresponding to 2.37 eV could be formed by the co-doping. The photocatalytic activity for nitrogen monoxide oxidation of SrTiO₃ in visible light region especially in the long wavelength range (λ > 510 nm) could be improved greatly. Under the irradiation of light with wavelength larger than 510 nm, the photocatalytic activity of nitrogen and sulfur co-doped SrTiO₃ was 10.9 times greater than that of pure SrTiO₃. The high visible light photocatalytic activity of this substance may be due to the formation of a new band gap that enables to absorb visible light effectively.