Quantitative information from x-ray diffraction of nylon-6 yarns. I. Development of a model for the analytical description of equatorial x-ray profiles

A wide-angle x-ray method has been developed by which quantitative structural information can be obtained on nylon-6 yarns. To this end, experimental equatorial diffractometer scans measured in transmission were fitted to a mathematical model describing the profiles as the envelopes of three bell-shaped functions. Four different models were investigated using, respectively, Gauss, Lorentz (Cauchy), Logistic, and Pearson-VII functions. The last model, which can be regarded as a generalized Lorentz function, gave the best fit. On the basis of a statistical analysis of the results of well-separated x-ray peaks, two parameters could be fixed. Another reduction of the number of parameters was achieved by interrelating the peak areas of the two outer reflections. These reductions widened the applicability of a computer program based on the aforementioned model to highly overlapping x-ray peaks. So the whole variety of x-ray scans, which can be obtained from nylon-6 yarns made under widely varying process conditions, can be well described. The fitting procedures provide unique solutions and hence objectively determined parameters.     

Mott-Schottky Analysis and Impedance Spectroscopy of TiO2/6T and ZnO/6T devices

Schottky junctions have been realized by evaporating gold spots on top of sexithiophen (6T), which is deposited on TiO 2 or ZnO with e-beam and spray pyrolysis. Using Mott-Schottky analysis of 6T/TiO2 and 6T/ZnO devices acceptor densities of 4.5x10(16) and 3.7x10(16) cm(-3) are obtained, respectively. For 6T/TiO2 deposited with the e-beam evaporation a conductivity of 9x10(-8) S cm(-1) and a charge carrier mobility of 1.2x10(-5) cm2/V s is found. Impedance spectroscopy is used to model the sample response in detail in terms of resistances and capacitances. An equivalent circuit is derived from the impedance measurements. The high-frequency data are analyzed in terms of the space-charge capacitance. In these frequencies shallow acceptor states dominate the heterojunction time constant. The high-frequency RC time constant is 8 micros. Deep acceptor states are represented by a resistance and a CPE connected in series. The equivalent circuit is validated in the potential range (from -1.2 to 0.8 V) for 6T/ZnO obtained with spray pyrolysis.     

Efficient, chemoenzymatic process for manufacture of the Boceprevir bicyclic [3.1.0]proline intermediate based on amine oxidase-catalyzed desymmetrization

The key structural feature in Boceprevir, Merck's new drug treatment for hepatitis C, is the bicyclic [3.1.0]proline moiety "P2". During the discovery and development stages, the P2 fragment was produced by a classical resolution approach. As the drug candidate advanced through clinical trials and approached regulatory approval and commercialization, Codexis and Schering-Plough (now Merck) jointly developed a chemoenzymatic asymmetric synthesis of P2 where the net reaction was an oxidative Strecker reaction. The key part of this reaction sequence is an enzymatic oxidative desymmetrization of the prochiral amine substrate.