The possibility of depositing copper powders with different apparent density by changing the shape of reversing current wave is shown. The morphology and crystallinity of powder particles can be varied considerably by changing shape of the reversing current wave and, hence, the apparent density of powders. The relation of apparent density with particle morphology and structure was illustrated.
An efficient, five-step synthetic approach to various acyclic 1,3-diamines has been developed and applied to the preparation of a novel class of open-chained fentanyl analogues. The acyclic derivatives 5.1?5.5 (all new compounds) were synthesized with the aim of estimating the significance of the piperidine ring for the opioid analgesic activity of anilido-piperidines. The starting ?-keto-amide 1.1, prepared by the aminolysis of methyl acetoacetate with methylphenethylamine, (93 % yield), was successively reacted with NaH and BuLi, to form the highly reactive ?,?-dienolate anion 1.1a. Regio and chemoselective ?-alkylation of the dienolate with various primary and secondary alkyl halides furnished the ?-keto-amides 1.2?1.5 (76?91 %). Reductive amination of the keto-amides 1.1?1.5 with aniline and Zn powder in acetic acid, via the enamine intermediates 2.1?2.5, afforded the ?-anilino amides 3.1?3.5 (74?85 %). After reductive deoxygenation of the tertiary amide group, using in situ generated diborane, the corresponding 1,3-diamines 4.1?4.5 were obtained (87?97 %). The synthesis of (?)-2,3-seco-fentanyls 5.1?5.5 was completed by N-acylation of the diamines 4.1?4.5 with propionyl chloride, followed by precipitation of the monooxalate salts (86?95 %). The parent compound, 2,3-seco-fentanyl 5.1, was found to be a 40 times less potent narcotic analgesic than fentanyl but still 5?6 times more active than morphine in rats, while i-Pr derivative 5.3 was inactive. Apart from the pharmacological significance, the general procedure described herein may afford various functionalized, 1,3-diamines as potential complexing agents and building blocks for the synthesis of aza-crown ethers.
One of the most important properties of copper powder is its flow ability which depends on the shape and the structure of the powder particles. A procedure for the determination of a representative powder particle permitting the free flow of copper powder is proposed.
The processes of Pb electrodeposition under diffusion control were examined by scanning electron microscopy (SEM) of the formed crystals. The orientation of grains of hexagonal shape formed in the initial stage of electrodeposition strongly affected the final morphology of the Pb crystals. The formation of Pb crystals of the different shape from the same initial shape was discussed in terms of the effect of orientation of initially formed grains on the type of diffusion control. A spherical diffusion layer was formed around the tip of the hexagonal-shaped grain oriented with its tip towards the bulk solution that led to the formation of elongated crystals in the growth process. On the other hand, a cylindrical type of diffusion was responsible for the growth of hexagonal-shaped grains oriented with the lateral side towards the bulk solution. Pb crystals with well-defined sides parallel to the surface area of the macroelectrode were formed under this type of diffusion.
The structure of the surface of copper powder particles is discussed and correlated with the lowest apparent density at which copper powder can still flow. It is shown that such structures can be easily obtained in the electrodeposition of powders in reversing current regimes.
An analysis of the effects of the shape, surface structure and size distribution of particles on the flow ability of the copper powder was performed. It is shown that the most important property of the particles of a powder, regarding the flow ability of the powder, is the surface structure of the particles.
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