Morphologies of microporous polyethylene and polypropylene crystallized from solution in supercritical propane

The morphologies of solvent-free, microporous, mechanically self-supporting cylinders of linear polyethylene and isotactic polypropylene, crystallized from solution in supercritical propane, were examined by an SEM technique. The morphology of gels (or foams), obtained with little or no shrinkage from 2% to 35% solutions by weight of polyethylene (99% to 85% porosities), is shown in some detail. Lamellae with very little or considerable mutual organization occur, often in the form of stacks with straight or coiled axes (axialites). Further growth of these can lead to particles with a roughly spherical overall shape and a predominantly radial orientation of the lamellae at the particle surface. Subcooled isotactic polypropylene, on the other hand, crystallizes in the form of perfectly shaped birefringent microspheres of very uniform size. ©1995 John Wiley & Sons, Inc.     

Crystal and molecular structure of 1R,3S,5S,7R,10R-3,6,6,10,14-Pentamethyltricyclo[10.3.0.05,7]pentadeca-11,14-diene-1, 10-dihydroxy-2,13-dione (Japodagrol), C20H28O4

A new cytotoxic macrocyclic diterpenoid named Japodagrol, C₂₀H₂₈O₄, has been isolated from the ornamental plantJatropha podagrica, family Euphorbiaceae, grown in Nigeria. The structure of the title compound, C₂₀H₂₈O₄, was solved by X-ray analysis.M _r =332.44, monoclinic space groupC2,a=23.285(4),b=6.5105(12),c=12.505(3) Å,=98.504(17),V=1874.8 ų,Z=4,D _c =1.178 Mg/m³. CuK radiation (graphite crystal monochromator, =1.54184 A), (CuK)=6.13 cm^–1,F(000)=720,T=290 K. Final conventionalR factor=0.035,R _w =0.038 for 3349 observed reflections. The structure was solved with the programDirdif. The 5-membered ring is closed to a half-chair form. The compound contains inter- and intramolecular hydrogen bonds.     

Gas chromatographic determination of estrone,estradiol and estriol in non-pregnancy plasma

Summary A gas Chromatographic method for the determination of estrone, estradiol and estriol in plasma of normal females is described. Purification is done by means of TLC of the free compounds and the acetates and quantitation is achieved by electron capture-gas chromatography of the estrogen heptafluorobutyrates. Experiments on the validation of the method are described along with some examples of its application.

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Zusammenfassung Eine gaschromatographische Methode zur Bestimmung von Östron, Östradiol und Östriol im normalen weiblichen Plasma wurde beschrieben. Die Reinigung erfolgte durch Dünnschichtchromatographie der freien Verbindungen und ihrer Acetate. Die quantitative Bestimmung wurde gaschromatographisch mit Hilfe eines Elektroneneinfangdetektors an Hand der Östrogenheptafluorobutyrate bewerkstelligt. Versuche zur Bewertung dieser Methode sowie Beispiele für ihre Anwendung wurden beschrieben.

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Supported by USPHS Grants AM 09908 and RCDA 5 K 3-AM-31, 321 (S. K.) and a grant from the Ford Foundation.     

ISOIREMCO 25 years of age (revisited)

Accreditation and Quality Assurance -     

Donor—acceptor interactions of substituted benzenes with molecular chlorine and carbon disulfide

CNDO molecular orbital calculations have been performed to analyze donor—acceptor interactions between molecular chlorine and benzene, toluene, mesitylene and hexamethylbenzene and the, as yet, unreported chlorine—hexafluorobenzene and carbon disulfide—benzene pairs. The stabilization energy and the dipole moment and its derivative (?p/?R_CICI) calculated for the benzene—chlorine complex are in good agreement with the estimated experimental values. The trends in the experimental stabilization energies and the Cl-Cl vibrational frequencies with increasing methyl substitution appear to be well reproduced by the calculations. The charge transferred from the benzene donor is polarized toward the outer chlorine atom or sulfur atom. For hexafluorobenzene-chlorine the direction of electronic charge polarization is reversed from that of the benzene and methylbenzene complexes. The calculated results are discussed within the framework of Muliiken's simplified resonance theory for complexes.     

Synthesis of a biotinated amphiphile

The synthesis of a biotinated amphiphile assembled from d-(+)-biotin, ethylene diamine as spacer, galactaric acid and 1-dodecylamine was achieved in six steps. The key step was the synthesis of a bisacetonide protected galactaric ester, the structure of which was determined by X-ray analysis. Aminolysis, spacer attachment, coupling with biotin and deprotection led to the amphiphilic galactaramide.     

Reactions of tetrahydro-as-triazine-3(2H)-thiories with α, β-difunctional compounds

The results of allowing tetrahydro-as-triazine-3(2H)-thiones to react with various α,β-diiunctional compounds, such as, α-bromoethyl p-toluenesulfonate, chloroacetaldehyde, α-bromophenylacet-uldehyde, phenaeyl bromide, chloroacetonitrile, α-bromophenylaeelonitrile, and α-cyanobenzyl p-toluenesulfonate are discussed. These condensations give either a 5H-thiazolo[3,2-b]-as-triazine or a 2H-thiazolo[2,3-c]-as-triazine.     

A 13C- and 195Pt-NMR. Study of the Complexes trans-PtCl2 (amine) (CH2CH2)

¹³C- and ¹⁹⁵Pt-NMR. spectra for the complexes trans-PtCl₂(amine)(CH₂?CH₂) have been measured. For amine = (S)-N-methyl-α-methylbenzylamine the two diastereomers present may be distinguished from the values ³J(Pt,C). The ¹⁹⁵Pt-chemical shift is shown to be sensitive to subtle differences stemming from intramolecular non-bonded interactions.