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1.
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. 相似文献
2.
A series of ethynyl and ethenyl end-capped imide resins were synthesised by the reaction of 9,9-bis(4-aminophenyl) fluorene
(BAF) with pyromellitic dianhydride (PMDA)3/3′, 4,4′-benzophenone tetracarboxylic acid dianhydride (BTDA)/2,2-bis(3,4-dicarboxy
phenyl) hexafluoropropane dianhydride (6F) and 3-ethynyl aniline/maleic anhydride. Structural characterisation was done by
infra red and elemental analysis. Thermal characterisation was done by differential scanning calorimetry and thermogravimetric
analysis. The decomposition temperatures of cured resins were above 200°C in nitrogen atmosphere. Char yield at 800°C ranged
from 59–65.5%. 相似文献
3.
The Pummerer reaction was carried out with α-acylsulfides and phenyl iodosyl bis(trifluoroacetate) instead of α-acylsulfoxides to prepare 4H-pyrrolo[2,1-c][1,4]benzothiazines and 3-(methyIthio)oxindoles. 相似文献
4.
E. A. Fedorova N. V. Glushkova M. N. Bochkarev H. Schumann H. Hemling 《Russian Chemical Bulletin》1996,45(8):1996-1999
Reactions of naphthaleneeuropium and naphthaleneytterbium, C10H8Ln(DME) (Ln = Eu or Yb), with phenylacetylene are accompanied by the formation of the C-C bond and yield the complexes of composition Ph2C4H2Ln(DME)2. Hydrolysis of the Ph2C4H2Ln(DME)2 complexes affords a mixture of isomers of 1,4-diphenyl-1,3-butadiene. Reactions of C10H8[LnI(DME)2]2 with PhCCH yield mixed iodine-ethynyl complexes [ILn(-CCPh)(DME)2]2. According to the data of X-ray diffraction analysis, the ytterbium complex consists of two YbI(DME)2 units bonded through two bridging CCPh groups. The crystals of this complex belong to the space groupP21/c. The central cyclic Yb-C-Yb-C fragment is planar; the C(I)-Yb(I)-C(I) angle is 86.4(3)°. The Yb-C bond lengths are 2.584(8) and 2.603(9) Å.Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 8, pp. 2101–2104, August, 1996. 相似文献
5.
Masayuki Hoshi Souichi Suzuki Shingo Saitoh Mitsuhiro Okimoto Kazuya Shirakawa 《Tetrahedron letters》2007,48(1):119-124
A convenient, efficient and stereoselective synthesis of a range of bis(alk-3-en-1-ynyl)benzenes with E- and Z-configuration is described. The protocol involves Cu-mediated cross-coupling reaction of (E)- and (Z)-alk-1-enyldisiamylboranes with (trimethylsilyl)ethynyl bromide and Pd/Cu-catalyzed cross-coupling reaction with diiodobenzene. The sequential cross-coupling reaction proceeds readily under extremely mild conditions in a one-pot manner to afford bis(alk-3-en-1-ynyl)benzenes in good to excellent yields. The optical properties of the products are also described. 相似文献
6.
Gui-Ling Zhao 《Tetrahedron》2005,61(30):7277-7288
This paper describes several highly efficient DABCO-catalyzed aza-Michael addition reactions of hydrazones to activated olefins. In most cases, these aza-Michael addition reactions gave the corresponding products in high yields under mild conditions. The plausible reaction mechanism is discussed on the basis of deuterium labeling experiments. Upon treatment with HCl, the corresponding cyclized products can be obtained in high yields from the Michael addition products. 相似文献
7.
Shushi Chen 《中国化学会会志》2003,50(6):1177-1182
The phenyl isothiocyanate, an electrophilic reagent for peptide chain sequencing, is used to pre‐column derivatize a variety of α‐amino acids in alkaline medium before their enantioresolution on a vancomycin bonded chiral phase using the acetonitrile‐based mobile phase. The observed resolution is believed to be due to the re‐location of the hydrogen receptor site from sulfur to nitrogen on the isothiocyanyl fragment of derivatizing reagent, which in turn changes the enantioselectivity. Under the same chromatographic conditions, the resolution for N‐benzoylated, 3,5‐dinitrobenzoylated and N‐carbobenzyloxylated amino acids is either not found or unsatisfactory. Also, no resolution is obtained in the reversed‐ or normal phase mode for all phenyl isothiocyanated amino acids examined in this study. 相似文献
8.
The reactions of 2-(1-hydropolyfluoro-1-alkenyl)-4H-3,1-benzoxin-4-ones (2) with hydrazine hydrate and phenyl hydrazine were investigated. The reaction of 2 with hydrazine hydrate in ethanol under reflux condition readily gave 2-fluoroalkyl-4H-pyrazolo[5,1-b]quinazolin-9-ones (3) in high yields. The reaction of 2 with phenyl hydrazine, however, resulted in the formation of 2-(2-phenyl-5-fluoroalkyl-2H-pyrazol-3-yl) benzoic acids (7). Further treatment of 7 with PPA gave 1-phenyl-4,9-dihydro-3-fluoroalkyl-1H-pyrozolo[3,4-b]quinolin-4-ones (4) in 65-80% overall yields. 相似文献
9.
D.I. Sánchez-Machado J. López-Cervantes J. López-Hernández P. Paseiro-Losada J. Simal-Lozano 《Chromatographia》2003,58(3-4):159-163
Summary A reversed-phase high-performance liquid-chromatographic method has been used for analysis of the amino acids in edible seaweed. Sample proteins were hydrolysed with hydrochloric acid and the amino acids produced were derivatized with phenyl isothiocyanate. The resulting phenylthiocarbamyl amino acids were chromatographed on an ODS2 column with UV detection at 254 nm. The mobile phase was a mixture of 0.14 M ammonium acetate buffer, pH 6.4, containing 0.05% triethylamine (A) and 60:40 (v/v) acetonitrile–water (B), at a flow rate of 1.1 mL min–1; the elution gradient (min:A%) was: 0:90, 8:90, 10:70, 12:70, 18:52, 20:0, 25:0, 28:90, 35:90. Method precision for the different amino acids was between 1.33 and 3.88% (relative standard deviation); detection limits were between 6.9 and 14.3 ng mL–1. The amino acid content of the algae analysed ranged from 22.4 ± 1.9 to 138.0 ± 5.6 mg g–1 d.w. The amino acids present at highest concentrations were glutamic acid, alanine, and phenylalanine. 相似文献
10.
Purification and reversible immobilization of d-amino acid oxidase from Trigonopsis variabilis could be simultaneously accomplished by hydrophobic interaction on Phenyl Sepharose CL-4B in the presence of 50 mM pyrophosphate buffer (pH 8.5). The presence of a high salt concentration of 2M, which is generally required for the hydrophobic interactions, was not essential for the hydrophobic immobilization. The
enzyme in free as well as immobilized form was optimally active between pH 7.0 and 9.0. The immobilized preparation could
be reused in a batch process for the conversion of d-amino acids to α-keto acids. When the activity of the preparation dropped below practical limits, the gel could be regenerated
by water wash and recharged with fresh crude extract from yeast. 相似文献