Transition‐metal‐catalyzed reactions of 5‐methylene‐2‐oxazolidinone and 5‐methylene‐1,3‐thiazolidine‐2‐thione with isocyanates

5‐Methylene‐2‐oxazolidinone (1) and 5‐methylene‐1,3‐thiazolidine‐2‐thione (4) react with various isocyanates to give the corresponding urethanes 3 and 5 in high yields in the presence of palladium(0) or palladium(II) catalyst under mild reaction conditions. A mechanism is proposed. Copyright © 2003 John Wiley & Sons, Ltd.     

Rhodium-catalyzed carbonylation of 2-alkynylbenzylamine: a new route to the synthesis of benzazepinones

Rhodium-catalyzed carbonylation of 2-alkynylbenzylamines under water-gas shift reaction conditions gives a seven-membered heterocyclic product, 2,4-disubstituted-1,4-dihydrobenz[c]azepin-3-ones, in a good yield.     

An Improved Synthesis of Retinoic Acid from β-Ionone

A convenient and large-scale preparation of retinoic acid 1 from β-ionone in five steps with 38% overall yield is described.The key steps are the epoxidization of 2 with a new methylated agent and the condensation 4 with tetraethyl methylenediphophonate in one-pot procedure to prepare 6.     

Kinetics and mechanism of the formation of poly[(1,1,3,3-tetramethyldisiloxanyl)ethylene] and poly(methyldecylsiloxane) by hydrosilylation

The kinetics of the formation of poly(carbosiloxane), as well as of alkyl-substituted poly(siloxane), by Karstedt's catalyst catalyzed hydrosilylation were investigated. Linear poly(carbosiloxane), poly[(1,1,3,3-tetramethyldisiloxanyl)ethylene], (PTMDSE), was obtained by hydrosilylation of 1,3-divinyltetramethyldisiloxane (DVTMDS) and 1,1,3,3-tetramethyldisiloxane (TMDS), while alkyl-substituted poly(siloxane), poly(methyldecylsiloxane), (PMDS), was synthesized by hydrosilylation of poly(methylhydrosiloxane) (PMHS) and 1-decene. To investigate the kinetics of PTMDSE formation, two series of experiments were performed at reaction temperatures ranging from 25 to 56 °C and with catalyst concentrations ranging from 7.0 × 10⁻⁶ to 3.1 × 10⁻⁵ mol Pt/mol CHCH₂. A series of experiments was performed at reaction temperatures ranging from 28 to 48 °C, with catalyst concentrations of 7.0 ×10⁻⁶ mol of Pt per mol of CHCH₂, when kinetics of PMDS formation was investigated. All reactions were carried out in bulk, with equimolar amounts of the reacting Si H and CHCH₂ groups. The course of the reactions was monitored by following the disappearance of the Si H bands using quantitative infrared spectroscopy. The results obtained showed typical first order kinetics for the PTMDSE formation, consistent with the proposed reaction mechanism. In the case of PMDS an induction period occurred at lower reaction temperatures, but disappeared at 44 °C and the rate of Si H conversion also started to follow the first-order kinetics. © 2007 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 45: 2246–2258, 2007     

Vapor-liquid equilibrium data at 25°C for six binary systems containing methyl acetate or methanol,with dichloromethane,chloroform, or 1,2-trans-dichloroethylene

Isothermal vapor-liquid equilibrium (VLE) data, at 25° C were determined by a saturation method for each of the six methanol or methyl acetate binary systems with dichloromethane, chloroform, and 1,2-trans-dichloroethylene. The experimental data satisfy the Redlich-Kister consistency test, and were correlated with five Gibbs free energy models. All the binary mixtures of methanol with the chlorinated compounds exhibit strong positive deviations from ideality while the mixtures of methyl acetate with the chlorinated compounds present negative deviations from ideal behavior.Communicated at the Festsymposium celebrating Dr. Henry V. Kehiaian's 60^th birthday, Clermont-Ferrand, France, 17–18 May 1990.     

Synthesis of polysiltrimethylenes with trimethylsilyl groups in the branch of the main chain

The thermally initiated and platinum-catalyzed polymerization of 1-silacyclobutanes with substitutents containing a trimethylsilyl group was carried out. Soluble, high-molecular-weight, heterochain siltrimethylene polymers were obtained, containing trimethylsilyl groups removed from the main chain by various bridges.A. V. Topchiev Institute of Petrochemical Synthesis, Russian Academy of Sciences, 117912 Moscow. Translated from Izvestiya Akademii Nauk, Seriya Khimicheskaya, No. 1, pp. 223–225, January, 1992.     

四溴双酚A锑铝双金属化合物的合成及其阻燃性能

以四溴双酚Ａ（ＴＢＡ）合成了在水和空气中稳定的四溴双酚Ａ合锑铝双金属化合物（ＴＢＡＳＡ）．通过ＩＲ、１ＨＮＭＲ和元素分析予以表征，并研究了其对聚乙烯（ＰＥ）和聚环氧乙烷（ＰＥＯ）的阻燃性能．结果表明，这种分子中含有溴、锑和铝的化合物，对聚乙烯和聚环氧乙烷等高聚物材料有高的阻燃性能与消烟效果．     

Solvothermal Synthesis of Molybdenum Disulfide Hollow Spheres Modified by Cyanex 301 in Water–Ethanol Medium

Hollow spherical molybdenum disulfide has been successfully synthesized via a solvothermal method using Cyanex 301 as sulfur source and modification agent. The hollow spheres are characterized by transmission electron microscopy, scanning electron microscopy, X-ray diffraction and Energy-Dispersive X-ray analysis. The influences of reaction conditions are also discussed while a mechanism is proposed to explain the formation of the peculiar morphology.     

Solvothermal synthesis of TiO2: anatase nanocrystals and rutile nanofibres from TiCl4 in acetone

This work reports a new synthetic approach for single‐phase TiO₂ nanomaterials by solvothermal treatment of titanium tetrachloride in acetone at 80–110 °C. Small, uniform, and yet size‐tunable (5–10 nm) anatase titania nanocrystallites were obtained using a low concentration of TiCl₄ in acetone (i.e., at molar ratios of TiCl₄/acetone ≤ 1:15) in the temperature range of 80–110 °C, while rutile nanofibers were synthesized using a high concentration of TiCl₄ (e.g., TiCl₄/acetone = 1:10) at 110 °C. Copyright © 2007 John Wiley & Sons, Ltd.