Analysis of the globins from fast human haemoglobins by isoelectrofocusing on polyacrylamide gel rods

The globins from all fast haemoglobin (Hb) components obtainable by Bio-Rex 70 cation-exchange chromatography were examined by isoelectrofocusing on polyacrylamide gel rods with 8.0 mol/l urea. From this analysis HbA1a1 and HbA1a2 seem to be very heterogeneous components. HbA1b is separable into two components, one of which is varied in both the beta chains. Between HbA1b2 and the well-known HbA1c components two chromatographic peaks are separated, one with a noticeable percentage of glucosylated beta chain and one that probably contains HbF. HbA1c has both beta chains glucosylated, while HbA1x seems to be a beta monoglucosylated Hb form. Finally, the early part of the HbAo peak has a large amount of glucosylation on both alpha and beta chains.     

The use of 18O substitution in the characterization of MReO4 molecules. The IR spectrum of matrix-isolated CsReO4

The molecular structure of gaseous CsReO₄ has been studied by matrix isolation IR spectroscopy. The ¹⁸O substitution experiments indicate a bidentate structure of C_2v symmetry in which the perrhenate anion is slightly distorted from the tetrahedral geometry.     

Radiation-induced crosslinking and grafting of two polyphosphazene elastomers

The radiation-induced crosslinking and grafting of two aryloxy-substituted elastomeric polyphosphazenes have been carried out by both gamma and electron beam irradiation. The classic Charlesby–Pinner [1] plus a simpler approach were used to determine the G(X) values for the crosslinked elastomeric polymers. The apparent G(X) value for the same polymer depended on whether the gamma-ray or the E-beam results were used. The presence of 8.5% repeat units with allylic groups in the side chain increased the G(X) value by an order of magnitude when the irradiation was performed under vacuum with the gamma source. The extent of acrylic acid grafting was also higher for the polymer containing the allylic group. Nearly all the grafted polyphosphazene films were insoluble in THF, a good solvent for the ungrafted samples.     

Synthesis of 1-alkyl(aralkyl)-4-acyl-2-piperazinones

1-Alkyl(aralkyl)-4-acyl-2-piperazinones are formed in high yields during selective acylation of N-monosubstituted ethylenediamines by benzoyl and cyclohexylcarbonyl chlorides in the presence of pyridine hydrochloride and treatment of the reaction products with chloroacetyl chloride in the presence of potassium tert-butylate.Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 4, pp. 514–517, April, 1986.     

Molecular structures of acetylene derivatives of tin: Part IV. Gas-phase electron-diffraction study of tetraethynyltin,Sn(CCH)4, and triethynyltin iodide,ISn(CCH)3

The geometrical parameters of tetraethynyltin and triethynyltin iodide have been determined by gas-phase electron diffraction. Triethynyltin iodide was present as an admixture in both the tetraethynyltin samples studied. Because the samples differed significantly in percentage of the iodide (17.4 ± 4.0 and 47.1 ± 3.5 mol %, in samples A and B, respectively), it was possible to determine the structures of both molecules to a sufficient degree of accuracy.The r_α, structures were solved by the least-squares treatment of the molecular intensities, using mean amplitudes and shrinkage corrections calculated from the force fields of a number of tin derivatives.The T_d-symmetry model of Sn(CCH)₄ was refined to give the following parameters: Sn-C, 2.068(5); CC, 1.228(8); CH, 1.079(51). The structural parameters for ISn(CCH)₃ (on the basis of the C_3v model with linear Sn-CC-H fragments) are as follows: Sn-I, 2.646(4); Sn-C, 2.062(17); CC, 1.226(6); ∠ISnC 108.0(2.8). (The thermal average bond distances, r_g, are given in Å, and the valence angle, rα, in degrees; the values in paren- theses are three times the standard deviations, 3σ.)The Sn-C bonds in Sn(CCH)₄, and ISn(CCH)₃ are shorter than the corresponding bonds in the monoethynyltin derivatives, Me₃SnCCH and Me₃SnCCSnMe₃. The SnI bond in ISn(CCH)₃ is noticeably shorter than those in stannane iodide and trimethylstannane iodide.     

Non planéité de cyclopenténones substituées analyse conformationnelle par résonance magnétique nucléaire

The stereochemistry of substituted cyclopent-2-en-1-ones was studied by NMR. The existence of non-planar rings is indicated and conformational analysis, based principally upon examination of the coupling constants enables the conformational population to be estimated; trans dihalogeno derivatives, for example, occur predominantly in the diaxial form.     

Synthesis and some properties of gem-dichlorocyclopropane carboxaldehyde acetals and cyclopropane carboxaldehyde acetals

α,β-Unsaturated aldehyde acetals add :CCl₂ (obtained in accordance with Makosza procedure) to form gem-dichlorocyclopropanecarboxaldehyde acetals (1) in high yields when the ratio of reactants is no less than 1:4. The addition of :CCl₂ to polyunsaturated aldehyde acetals in the above conditions proceeds regioselectively at double bonds enriched by electrons. Compounds 1 are reduced by sodium in liquid ammonia to give cyclopropanecarboxaldehyde acetals (2). Both 1 and 2 are hydrolized by dilute H₃P0₄ to the corresponding aldehydes and are added to vinyl ethers in the presence of BF₃·Et₂O to produce only 1:1 adducts which are hydrolyzed by a mixture of AcOH-AcONa-H₂O to give β-formylcyclopropanes which were previously unknown.     

Anionic polymerization of 1,2-butylene oxide

Anionic polymerizations of 1,2-butylene oxide were carried out in vacuum-sealed dilatometers in the range of 30–60°C. Potassium terbutoxide and dimsyl sodium were used as initiators; dimethyl sulfoxide (DMSO) and mixtures of DMSO with tetrahydrofuran were solvents. The polymer products were analyzed by gel permeation chromatography and infrared spectroscopy. The object of the investigation was to obtain information on the mechanism of the reaction and to elucidate some of its kinetic aspects. It has been shown that the polymerizations occur by two different processes, depending on the choice of experimental conditions. One of the processes involves free ions and ion-pairs, the other, ion-pairs alone. In the first case, where dimethyl sulfoxide is used as solvent, the order of the reaction with respect to the initiator concentration far exceeds unity (～1.8), while in the second case, involving mixed solvents, the order of the reaction, for all practical purposes, is one.     

Derivative Dilatometrie

Zusammenfassung Die derivatographische Methode wurde weiterentwickelt. Mit Hilfe einer neuen Einrichtung kann man die Temperatur, die Gewichtsänderung und die Dilatation der Probe sowie auch die Geschwindigkeit der Enthalpie- und Gewichtsänderungen und die Geschwindigkeit der Dilatation messen. Die Vorteile der Einrichtung wurden an einigen praktischen Beispielen erläutert.

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Summary The derivatographic method was further developed. With the aid of a new apparatus it is possible to measure the temperature, the change in weight and the dilatation of the sample, as well as the velocity of the changes; in enthalpy and weight and the velocity of the dilatation. The advantages of the apparatus were demonstrated by means of several practical examples.

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Résumé On a élargi le domaine des méthodes dérivatographiques. A l'aide d'un nouveau dispositif, on peut mesurer la température, la variation de poids et la dilatation de l'échantillon, ainsi que la vitesse des changements d'enthalpie et de poids, et aussi la vitesse de la dilatation. On a montré les avantages de ce dispositif sur un certain nombre d'exemples pratiques.

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Bei der Ausführung der Versuche waren uns FrauM. Csonka und FrauE. Borsay behilflich, wofür wir ihnen auch an dieser Stelle danken.