Synthesis of some phosphonocarbonyl compounds via Horner-Emmons reaction of methylenbisphosphonate

Summary The -carbonyl substituted vinylphosphonates6–9 were synthesized from the -dicarbonyl compounds2–5 and the methylenbisphosphonate1 by a Horner-Emmons reaction in different yields.

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Synthese von Phosphonocarbonylverbindungen durch Horner-Emmons-Reaktion von Methylenbisphosphonsäuretetraethylester

Zusammenfassung Es wurden die -carbonylsubstituierten Vinylphosphonate6–9 mittels Horner-Emmons-Reaktion aus den -Dicarbonylverbindungen2–5 und Methylenbisphosphonat1 in verschiedenen Ausbeuten hergestellt.

     

Synthesis and structure of novel derivatives of thieno[2,3-b]thiocine. An unusual product of intramolecular cycloaddition of 2-homomethallylthio-5-methyl-3-thiophenecarbonitrile oxide

9-Methyl-3,3a,4,5-tetrahydro-6H-thieno[2,3-b]thiocino[4,5-c]isoxazole and 9-hydroxyimino-2-methyl-7-methylene-6, 7,8,9-tetrahydro-5H-thieno[2,3-b]thiocine have been prepared for the first time by the oxidation of 2--alkenylthio-3-thiophenecarbaldoximes with NaOCl. X-ray structural investigations of thieno[2,3-b]thiocine and 2-homomethallylthio-5-methyl-3-thiophenecarbaldoxime have been carried out.Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 7, pp. 1262–1266, July, 1993.     

The search for a new model structure of β-Factor XIIa

We present the search for a new model of -factor XIIa, a blood coagulation enzyme, with an unknown experimental 3D-structure. We decided to build not one but three different models using different homologous proteins as well as different techniques and different modellers. Additional studies, including extensive molecular dynamics simulations on the solvated state, allowed us to draw several conclusions concerning homology modelling, in general, and -factor XIIa, in particular.     

Structure-Activity Relationship of Insecticidal Steroids. III. Δ4,7-6-Ketosteroids

The toxicity of steroids 1-11 for colorado beetle (Leptinotarsa decemlineata Say.) larvae was studied by contact-intestinal treatment. Active insect-growth regulators were found among the studied compounds.     

Thermal degradation behaviors of some branched and linear polysiloxanes

The thermal degradation behaviors of some branched and linear polysiloxanes were studied by thermogravimetric (TG) analysis and infrared (IR) spectroscopy, and the effect of phenyl content on the thermal stability of the tested branched polysiloxanes was investigated. The branched polysiloxanes with phenyl obtain higher thermal stability at lower temperature. The degradation residues of the examined branched polysiloxanes at 800 °C are rather high, 65.1-77.6% in N₂ and 40.5-66.5% in air, respectively. However, the amount of solid residue increases with decrease in phenyl content in both N₂ and air atmospheres. It was found that the thermal stability of the branched polysiloxanes is higher than that of the linear one, which indicated that the branched structure benefits the formation of a crosslink in the solid residue.     

紫外分光光度法测定甲砜霉素片的含量

根据甲砜霉素的紫外吸收特征,建立了以乙腈-水为溶媒、(225±1)nm为最大吸收波长的紫外分光光度法。方法的线性范围为0.5～25.0μg/mL,平均回收率为99.92％,RSD为0.30％。用对照品比较法测定5批甲砜霉素片的含量,并与中国药典方法的测定结果进行比对,结果表明,两种方法的测定结果基本一致。     

A new biodegradable polydepsipeptide microsphere for application in drug delivery systems

A sequential polydepsipeptide containing a tripeptide sequence L-alanyl-Lalanyl-ethyl L-glutamyl and an-hydroxy acid L-lactic acid, poly(Ala-Ala-Glu(OEt)-Lac), was synthesized to prepare the microspherical particles by the solvent evaporation process. In this case, the solvents play the most important role for the preparation of polydepsipeptide microspheres and, as an example, when 200 mg of the polydepsipeptide dissolved in 10 ml of 98/2% chloroform/dichloroacetic acid mixture was stirred at 400 rpm and 30 C, the microspherical particles with mean diameter of 58m were formed after pouring into 200 ml of 1% (w/v) poly(vinyl alcohol) solution. 17-Estradiol was incorporated into the particles, and the resulting particles were found to contain 5 mg of drug per 25 mg of the particle. The in vivo release of drug from the microspherical formulation was evaluated by measuring the pharmacological influence on rat prostate. It was found that the sufficient amount of drug, keeping the effective pharmacological influence, is supplied during the first 12-week period, followed by an incomplete supplying of drug intil the implant is perfectly degraded in vivo in the 25th week from the start of implantation.     

Boron chelates with 5,5,5-trifluoro- and 5,5,5-trichloro-4-aminopent-3-en-2-ones

Boron chelates were obtained by the reaction of butoxy(butylthio)diphenylborane with 5,5,5-trifluoro(trichloro)-4-aminopent-3-en-2-one, and their reactions with primary amines were investigated. -Diiminate complexes of boron with trifluoro- and trichloromethyl groups were synthesized.N. D. Zelinskii Institute of Organic Chemistry, Russian Academy of Sciences, 117913 Moscow. Translated fromIzvestiya Akademii Nauk, Seriya Khimicheskaya, No. 11, pp. 2657–2661, November, 1992.     

Liquid chromatography of the s-triazines

Summary A series of thirty s-triazine compounds have been separated using reversed-phase high-pressure liquid chromatography. A relationship between substituent activity and retention time was developed to predict molecular structure.Work partially completed at the CIBA-GEIGY Corp., McIntosh, Ala., USA.