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  • 1
    ISSN: 0018-019X
    Keywords: Chemistry ; Organic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The title compounds 6 and 7 have been prepared from the known 2,3-di-O-benzyl-4,6-O-benzylidene-D-galactose (18) and N2-acetyl-tri-O-benzyl-D-glucosamine oxime (29) in eight and six steps, respectively. The azidonitrile leading to the benzylated galacto-tetrazole 16 was prepared from 14 and cyclized under the conditions of its formation (Scheme 1). The alcohol 13 was obtained by oxidation of 10 followed by reduction. Better yields and diastereoselectivities were realized, when the benzylidene-protected D-galacto-alcohol 20 was subjected to oxido-reduction, yielding the L-altro-alcohol 22 via the ketone 21 (Scheme 2). Treatment of the corresponding tosylate 24 with NaN3 yielded the tetrazole 25, which was deprotected to 6. The tetrabenzyl ether 16 (from 14, or from 25 via 27) was reduced to 28 and deprotected to give the known deoxygalactostain 8 (Scheme 2). Oxidation of the hydroxynitrile 30, derived from 29, followed by reduction of 32 yielded mostly the L-ido-hydroxynitrile (Scheme 3), which was tosylated and treated with NaN3 to give the tetrazole 35a and its manno-isomer 36a, while Al(N3)3 yielded (E)- and (Z)-38 (Scheme 4). The intermediate azide 39 was isolated besides 40 when NH4N3/DMF was used; thermolysis of 39 gave mostly 35a, which was deprotected to 7, besides some elimination product 41. Both 6 and 7 are stable in the pH range 1-10; at pH 12, 6 is unaffected but, 7 shows some epimerization to the manno-configurated isomer 43. The tetrazole 6 is a competitive inhibitor of the β-galactosidases from E. coli (K1 = 1 μM, pH 6.8) and bovine liver (K1 = 0.8 μM, pH 7.0); the N-acetyl-β-D-glucosaminidase from bovine kidney is competitively inhibited by 7 (K1 ≊ 0.2 μM, pH 4.1).
    Additional Material: 1 Tab.
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  • 2
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 125 (1992), S. 3-7 
    ISSN: 0009-2940
    Keywords: Indium, pentacoordinated organo compounds ; Intramolecular base stabilization ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Synthesis and X-ray Structural Analysis of Airstable Bis[3-(dimethylamino)propyl]indium DerivativesPentacoordinate, intramolecularly base-stabilized organoindium compounds [Me2N(CH2)3]2InBr (1), [Me2N(CH2)3]2InO2-CCF3 (2) and [Me2N(CH2)3]2InOC6F5 (3) as well as [Me2N-(CH2)3]2InC2H5 (4), [Me2N(CH2)3]2In(i-C3H7) (5), and [Me2N-(CH2)3]2In(t-C4H9) (6) have been prepared by the reaction of indium tribromide with 3-(dimethylamino)propyllithium and of bis[3-(dimethylamino)propyl]indium chloride with NaO2C-CF3, LiOC6F5, C2H5MgBr, i-C3H7MgBr, and t-C4H9Li, respectively. The 1H-, 13C-, 19F-NMR and mass spectra of the new compounds as well as the single-crystal X-ray structure analysis of 1 are described and discussed.
    Additional Material: 2 Ill.
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  • 3
    ISSN: 0269-3879
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: Racemic phenylpropanolamine was resolved on a high performance liquid chromatographic (HPLC) chiral stationary phase (CSP) as the 3,5-dinitrophenyl ureide derivative. The CSP was prepared by a simple in situ procedure in which (R)-(1-naphthyl)ethyl isocyanate was bound to aminopropyl silanized silica through a urea linkage. The enantiomeric ureides were prepared by a room-temperature, 60-second procedure, accomplishing simultaneous extraction and derivatization and utilizing achiral 3,5-dinitrophenyl isocyanate as reagent. Baseline resolution was readily achieved under normal phase conditions, with a separation factor (α) of 1.16 and a resolution factor (Rs) of 2.2. Elution was complete within 10 min. A limit of detection, by UV at 235 nm, of 250 pg per isomer was established. Feasibility of the procedure for plasma determinations was demonstrated by assay of samples from a canine subject.
    Additional Material: 2 Ill.
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  • 4
    Electronic Resource
    Electronic Resource
    New York, NY [u.a.] : Wiley-Blackwell
    Journal of Applied Polymer Science 21 (1977), S. 1189-1197 
    ISSN: 0021-8995
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Physics
    Notes: In previous papers, interpenetrating polymer networks were shown to display a cellular structure. The phase domain size of polymer II was shown to depend inversely on the crosslink density of polymer I. The present paper presents a semiempirical derivation of equations which show quantitatively the dependence of the phase domain size of polymer II on the crosslinking density of polymer I, and also on the interfacial energy and the overall composition. If polymer II is linear, the dependence on the molecular weight of polymer II is also included. The values of the phase domain sizes so estimated are compared with experimental results. While theory and experiment yield good agreement, the semiempirical nature of the equations must be borne in mind.
    Additional Material: 2 Ill.
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  • 5
    Electronic Resource
    Electronic Resource
    New York, NY [u.a.] : Wiley-Blackwell
    Journal of Applied Polymer Science 26 (1981), S. 591-602 
    ISSN: 0021-8995
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Physics
    Notes: Reticulated polystyrene-divinylbenzene (PSt-DVB) copolymer membranes or thin sheets were prepared using two different methods. The first method employed a nonsolvating diluent which dissolves the monomer but precipitates the polymer. This resulted in skinned membranes with the skin being nonporous, being either crenelated or smooth. The second method used paraffin wax as the inert phase. The wax was precipitated by cooling, followed by polymerization of the styrene. The wax was then solvent extracted. This resulted in a reticulated structure both on the surface and in the interior of the membrane. The resulting products from the two methods were compared using scanning electron microscopy. The objective of this study was to prepare a skinless, macroporous, crosslinked polystyrene, as polymer I for the preparation of novel interpenetrating polymer network (IPN) materials.
    Additional Material: 7 Ill.
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  • 6
    Electronic Resource
    Electronic Resource
    New York, NY [u.a.] : Wiley-Blackwell
    Journal of Applied Polymer Science 34 (1987), S. 409-422 
    ISSN: 0021-8995
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Physics
    Notes: Areas under the linear tan δ-temperature (tA) and linear loss modulus-temperature (LA) curves of the polyacrylate and polymethacrylate homologous series and their interpenetrating polymer networks (IPNs) were investigated. For poly(methyl acrylate), LA values are independent of crosslinking level through 25%, but tA decreases. With increasing side group length, on the other hand, tA remains nearly independent of side group length for both homologous series, having values near 50 and 65 (units of K) for the acrylate and methacrylate series, respectively. However, LA decreases steeply with increasing side group length. A phenomenological treatment of areas is presented in order to explain tA and LA behavior semiquantitatively. Both tA and LA exhibit areas characteristic of the structure of the particular polymers. The homopolymer LA areas are additive in determining the area under the corresponding curve for the IPN. This suggested a group contribution analysis for LA, where each moiety contributes specific values to the area.
    Additional Material: 9 Ill.
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  • 7
    Electronic Resource
    Electronic Resource
    New York, NY [u.a.] : Wiley-Blackwell
    Journal of Applied Polymer Science 33 (1987), S. 2637-2645 
    ISSN: 0021-8995
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Physics
    Notes: Novel acrylic/methacrylic interpenetrating polymer networks (IPNs) were examined by dynamic mechanical spectroscopy for their damping capabilities. While simple homopolymers exhibit high damping properties only over a 20-30°C range, multicomponent polymer systems with controlled degree of miscibility, such as IPNs, may exhibit high damping properties over temperature ranges as broad as approximately 100°C. Two series of IPNs based on poly(n-butyl acrylate) and poly(n-butyl methacrylate) were synthesized and the dynamic mechanical properties were investigated using a Rheovibron. Graphite was incorporated into the poly(n-butyl acrylate) homopolymer and a few IPNs to measure the change in the damping properties. For important IPN compositions, tan δ values between 0.4 and 0.85 were observed over a 75°C plus temperature range. Graphite increased the damping properties of poly(n-butyl acrylate) and the IPNs, as indicated by the tan δ values.
    Additional Material: 5 Ill.
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  • 8
    Electronic Resource
    Electronic Resource
    New York, NY [u.a.] : Wiley-Blackwell
    Journal of Applied Polymer Science 5 (1961), S. 527-533 
    ISSN: 0021-8995
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Physics
    Notes: A system is described for automatic collection of stress-strain data for polymeric films on magnetic tape for subsequent automatic data reduction and computation of a variety of stress-strain parameters. Two shaft analog-to-digital encoders attached to a conventional tensile tester feed digital information to an incremental pulse recorder which stores all stress and strain data in two channels on 0.625-in. magnetic tape. Specimen information and test constants are inserted by the operator through a keyboard located at the tensile tester. The tape is subsequently fed into a standard digital computer through a special incremental pulse magnetic tape reader. The data pulses are internally stored and converted by means of a special program into eight significant stress-strain parameters for polymeric film samples, plus averages and standard deviations for groups of replicate determinations. These parameters include: corrected length of specimen, initial maximum tensile modulus, offset yield stress, strain at break, strain at maximum stress, maximum tensile stress, tensile stress at break, and work to break. While the program described applies to polymer film testing, both it and the digital recording equipment accessories are applicable with suitable modification, to any analog experimental data. Significant savings in man-hours and increased information output result from use of this system.
    Additional Material: 5 Ill.
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  • 9
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A comparative mass spectral examination of the trimethylsilyl (TMS) derivatives of 2′-, 3′- and 5′-deoxyadenosine, 2′-, 3′- and 5′-deoxyguanosine, 2′-, 3′- and 5′-deoxyxanothosine and 2′- and 5′-deoxy-2-fluoroadenosine is presented. A general compilation of the major fragment ions found in the low-resolution electron ionization (EI) spectra of the eleven deoxynucleosides is given. Chemical ionization (CI)-collisional activation (CA) daughter ion spectra are reported using the deoxyadenosines as model compounds. Ion structures and fragmentation pathways are proposed for those ions characteristic of each of the isomers. Significant differences in fragmentation exist between the isomeric 2′-, 3′- and 5′-purine deoxynucleosides. The formation and structures of ten ions important in this differentiation are discussed. The CI-CA linked scan spectra provide complementary structural information relative to the EI mass spectra.
    Additional Material: 3 Ill.
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  • 10
    Electronic Resource
    Electronic Resource
    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part A: Polymer Chemistry 31 (1993), S. 749-753 
    ISSN: 0887-624X
    Keywords: chitin ; chitosan ; degree of N-acetylation ; near infrared spectroscopy ; calibration ; 2-acetamido-2-deoxy-D-glucopyranose ; 2-amino-2-deoxy-D-glucopyranose ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Chitin and its derivative chitosan are rapidly becoming of commercial interest in the biomedical, wastewater treatment, and fiber industries. One of the most important properties of these copolymers is the degree of N-acetylation. Presently there is no rapid accurate method to determine this value. We propose near infrared spectroscopy for such a method. Using a primary method such as hydrobromic acid titration or 1H-NMR, standards can be established. Once a model calibration equation has been developed, unknown samples can be analyzed by near infrared spectroscopy in less than 5 min. This is demonstrated by examining representative structural monomers of chitosan, N-acetyl-D-glucosamine and D-glucosamine hydrochloride, as model compounds as well as actual chitin and chitosan samples. © 1993 John Wiley & Sons, Inc.
    Additional Material: 6 Ill.
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