Novel synthesis of the ocular age pigment A2-E: new method for substituted pyridine synthesis via azaelectrocyclization

[reaction: see text] The formal synthesis of the ocular age pigment A2-E was achieved by the efficient one-pot preparation of the substituted pyridine, which involves the aza-6pi-electrocyclization of the Schiff base derived from (E)-3-carbonyl-2,4,6-trienal followed by oxidation.     

Surface Modification of Fine Particles with a SnO<Subscript>2</Subscript> Film by Using a Polyhedral-Barrel Sputtering System

Fine particles were modified with a thin film of SnO₂ by using a barrel sputtering system that is a dry process. The conditions for the preparation of SnO₂ were studied by reactive sputtering onto a glass plate substrate. The optimal conditions for the preparation of tetragonal SnO₂ were identified as 60% partial oxygen pressure and 1.0 Pa total gas pressure with the substrate at room temperature. Under the optimized conditions, the surfaces of Al flake particles were modified with a thin film of SnO₂. XRD and SEM/EDS analysis of the prepared samples showed that the Al particle surfaces were uniformly modified by a thin film of SnO₂ in all cases. The film thicknesses were 80, 130, and 180 nm at RF outputs of 195, 350, and 490 W. These measured thicknesses coincided with the values estimated from the interference colors of the samples.     

Studies on the synthesis of condensed pyridazine derivatives. IV. Synthesis and anxiolytic activity of 2-aryl-5,6-dihydro-(1)benzothiepino[5,4- c]pyridazin-3(2H)-ones and related compound.

A series of 2-aryl-5,6-dihydro-(1)benzothiepino[5,4-c]pyridazin-3(2H)- ones and related compounds were synthesized and evaluated for their ability to displace 3H-diazepam from rat brain membranes in vitro, and to prevent bicuculline induced convulsions in mice in vivo. Compounds with a 4'-methoxyphenyl (36) or 4'-chlorophenyl group (37, 39--42) as 2-aryl substituents showed prominent activities in both the in vitro and in vivo tests. Among them, 2-(4'-chlorophenyl)-5,6-dihydro- (37) and 2-(4'-chlorophenyl)-5,6-dihydro-10-fluoro-(1)benzothiepino[5,4-c]+ ++pyridazin- 3(2H)-one 7-oxides (41) showed activity twice as potent as diazepam in an anticonflict test (Vogel type, rats) while exhibiting less muscle relaxation (rotarod test, mice) and augmentation of gamma-aminobutyric acid-induced chloride current (Icl) in isolated frog sensory neurones than diazepam. Compound 37 (Y-23684) was selected from this series as a candidate for further development. The structure-activity relationships are discussed.     

Fluorescence modification of Gb3 oligosaccharide and rapid synthesis of oligosaccharide moieties using fluorous protective group

The use of the bisfluorous chain-type propanoyl (Bfp) group as a fluorous protective group made it possible to rapidly synthesize the Gb2 and Gb3 oligosaccharide derivatives by a simple fluorous-organic extraction purification. Furthermore, the fluorescence-labeled Gb2 and Gb3 oligosaccharides were prepared as a potential Vero Toxins detecting reagent.     

Isolation of o-xylylene (o-quinodimethane) dirivatives. A strong through-bond interaction in 2,3-benzobicyclo[2.2.0]hexane system

Some o-xylylene (o-quinodimethane) derivatives were isolated as stable cyrstalline materials. A strong through-bond interaction in tetracyanoethylene addition product of tetraphenylbenzodicyclobutadiene ($\text{21}$ is suggested.     

Preparation and thermal analysis of synthetic malachite CuCO3·Cu(OH)2

The synthesis of malachite CuCO₃·Cu(OH)₂ or Cu₂CO₃(OH)₂ was studied through titrations of copper(II) salt solutions with a solution of sodium carbonate at different temperatures. The precipitates were characterized by TG, IR and chemical analysis. The composition varies depending on thepH of the solution and the temperature. Purer malachite was synthesized by simple mixing of a solution of copper(II) nitrate or sulfate with a solution of sodium carbonate at 50°C.The kinetics of the thermal decomposition of synthetic malachite was described by eitherR ₃ orA _m(m=1.2–1.4) law, according to TG analysis, both isothermal and nonisothermal. The Arrhenius parameters determined using three different integral methods showed the kinetic compensation effect, which is correlated to the working temperature interval analyzed.The authors thank Mr. H. Takemoto for analyzing kinetics of the thermal decomposition of synthetic malachite.