Enantioselective synthesis of cocaine C-1 analogues using sulfinimines (N-sulfinyl imines)

The first examples of cocaine analogues having substituents (methyl, ethyl, n-propyl, n-pentyl, and phenyl) at the C-1 position of the cocaine tropane skeleton were prepared by heating sulfinimine-derived α,β-unsaturated pyrrolidine nitrones. In the presence of the Lewis acid Al(O(t)Bu)(3) the nitrones undergo an intramolecular [3 + 2] cycloaddition to give tricyclic isoxazolidines that were transformed in three steps to the cocaine analogues. In the absence of the Lewis acid, lactams were formed resulting from rearrangement of the nitrone to an oxaziridine. A novel Pd- and base-promoted rearrangement of methanesulfonate salts of isoxazolidine to bridge bicyclic[4.2.1]isoxazolidines was discovered.     

Phase transformation and crystallization kinetics of melt-spun Ni60Nb20Zr20 amorphous alloy

The glass transition and crystallization kinetics of melt-spun Ni₆₀Nb₂₀Zr₂₀ amorphous alloy ribbons have been studied under non-isothermal and isothermal conditions using differential scanning calorimetry (DSC). The dependence of glass transition and crystallization temperatures on heating rates was analyzed by Lasocka's relationship. The activation energies of crystallization, E_x, were determined to be 499.5 kJ/mol and 488.6 kJ/mol using the Kissinger and Ozawa equations, respectively. The Johnson–Mehl–Avrami equation has also been applied to the isothermal kinetics and the Avrami exponents are in the range of 1.92–2.47 indicating a diffusion-controlled three-dimensional growth mechanism. The activation energy obtained from the Arrhenius equation in the isothermal process was calculated to be E_x = 419.5 kJ/mol. The corresponding three dimensional (3D) time–temperature–transformation (TTT) diagram of crystallization for the alloy has been drawn which provides the information about transformation at a particular temperature. In addition, the intermetallic phases and morphology after thermal treatment have been identified by X-ray diffraction (XRD) and scanning electron microscope (SEM).     

Effect of laser melting on plasma-sprayed aluminum oxide coatings reinforced with carbon nanotubes

The effect of laser melting on the microstructure and mechanical properties of plasma-sprayed aluminum oxide composite coating reinforced with 4 wt% multi-walled carbon nanotubes (CNTs) is reported. Laser-melted layer consists of dense, coarse columnar microstructure which is significantly different from plasma-sprayed coating that consists of splats and porosity. CNTs retained their original cylindrical graphitic structure after undergoing laser irradiation. Three dimensional heat flow model has been developed to estimate temperature variation in the laser-melted composite layer. Laser-melted layers show an increase in the microhardness at the expanse of degradation of fracture toughness. Nanoindentation study indicates an increase in the elastic modulus and yield strength of the laser-melted layer which is attributed to dense microstructure with absence of weak-bonding splats and porosity.     

A Validated,Stability-Indicating HPTLC Method for Analysis of Doxofylline

JPC – Journal of Planar Chromatography – Modern TLC - A simple, sensitive, selective, precise, and stability-indicating high-performance thin-layer chromatographic method for analysis...     

Microstructure and properties of spark plasma sintered Fe–Cr–Mo–Y–B–C bulk metallic glass

Fabrication of Fe-based amorphous alloy using spark plasma sintering (SPS) process has been reported. Fully amorphous compacts with ～95% relative density were successfully sintered at temperature about 100 °C lower than glass transition temperature (T_g: 575 °C). Formation of crystalline Fe₂₃(C, B)₆ phases within near-fully dense (～99%) amorphous matrix is observed at sintering temperatures (>550 °C) close to glass transition temperature. Microstructure evolution in sintered compacts indicated that density, degree of crystallinity, and mechanical properties can be effectively controlled by optimizing SPS parameters.     

Energy levels and radiative rates for Ne-like ions from Cu to Ga

Energy levels, lifetimes and wave function compositions are computed for 127 fine structural levels in Ne-like ions (\(Z=29{-}31\)). Configuration interaction has been included among 51 configurations (generating 1016 levels) and multiconfigurational Dirac–Fock method is used to generate the wave functions. Similar calculations have also been performed using the fully relativistic flexible atomic code (FAC). Transition wavelength, oscillator strength, transition probabilities and line strength are reported for electric dipole (E1), electric quadrupole (E2), magnetic dipole (M1) and magnetic quadrupole (M2) transitions from the ground level. We compared our calculated results with the available data in the literature. The calculated results are found to be in close agreement with the previous results. Further, we predict some new atomic data which may be important for plasma diagnostics.     

Hydrogen Bonded Channel Formation in a Molecular Complex: <Emphasis Type="Italic">cis-</Emphasis>1-Chloro-2-ammonium-1-trimethylsilylcycloheptane Picrate

Abstract  The crystal and molecular structure of cis-1-chloro-2-amino-1-trimethylsilylcycloheptane picrate (cis-CATP) is determined and discussed along with its spectroscopy. The crystal structure of this compound (C₁₀H₂₃SiClN⁺ C₆H₂N₃O₇⁻) consists of ammonium cycloheptane cation and picrate anion stabilized by interionic N–H···O and C–H···O interactions leading to extended hydrogen bonded network structure. Apart from the less common syn addition of nitrosylchloride to 1-trimethylsilylcycloheptene ring, an interesting and unexpected reversal of regiochemistry of addition is revealed. Index Abstract  The preparation of cis-1-chloro-2-ammonium-1-trimethylsilylcycloheptane picrate is described and its crystal structure is determined and discussed.      

On a mild generalization of the Schönemann - Eisenstein - Dumas irreducibility criterion

We state a mild generalization of the classical Schönemann and Eisenstein- Dumas irreducibility criterion in ?[x] and provide an elementary proof. In the end of the paper, we also provide a concrete example of a polynomial which is irreducible by the main result of the paper but whose irreducibility does not follow from existing criteria.     

On integrally closed simple extensions of valuation rings

Let v be a Krull valuation of a field with valuation ring $R_v$. Let θ be a root of an irreducible trinomial $F(x)=x^n+a{x}^m+b$ belonging to $R_v[x]$. In this paper, we give necessary and sufficient conditions involving only $a,b,m,n$ for $R_v[\theta ]$ to be integrally closed. In the particular case when v is the p-adic valuation of the field $\mathbb{Q}$ of rational numbers, $F(x)\in \mathbb{Z}[x]$ and $K=\mathbb{Q}(\theta )$, then it is shown that these conditions lead to the characterization of primes which divide the index of the subgroup $\mathbb{Z}[\theta ]$ in $A_K$, where $A_K$ is the ring of algebraic integers of K. As an application, it is deduced that for any algebraic number field K and any quadratic field L not contained in K, we have $A_{KL}=A_K{A}_L$ if and only if the discriminants of K and L are coprime.     

On the compositum of integral closures of valuation rings

It is well known that if $K_1,K_2$ are algebraic number fields with coprime discriminants, then the composite ring $A_{K_1}{A}_{K_2}$ is integrally closed and $K_1,K_2$ are linearly disjoint over the field of rationals, $A_{K_i}$ being the ring of algebraic integers of $K_i$. In an attempt to prove the converse of the above result, in this paper we prove that if $K_1,K_2$ are finite separable extensions of a valued field $(K,v)$ of arbitrary rank which are linearly disjoint over $K=K_1\cap K_2$ and if the integral closure $S_i$ of the valuation ring $R_v$ of v in $K_i$ is a free $R_v$-module for $i=1,2$ with $S_1{S}_2$ integrally closed, then the discriminant of either $S_1/R_v$ or of $S_2/R_v$ is the unit ideal. We quickly deduce from this result that for algebraic number fields $K_1,K_2$ linearly disjoint over $K=K_1\cap K_2$ for which $A_{K_1}{A}_{K_2}$ is integrally closed, the relative discriminants of $K_1/K$ and $K_2/K$ must be coprime.