Synthesis and reactions of 2‐chloro‐2‐(hydroximino)‐1‐(4‐methyl‐2‐phenylthiazol‐5‐yl)ethanone

3‐Nitrosoimidazo[1,2‐a]pyridine, 3‐nitrosoimidazo[1,2‐a]pyrimidine, 3‐nitrosoquinoxaline, 2‐nitroso‐4H‐benzo[b]thiazine, 2‐nitroso‐4H‐benzo[b]oxazine, isoxazoles, isoxazolo[3,4‐d]pyridazines and pyrrolo[3,4‐d]isoxazole‐4,6‐dione were synthesized from 2‐chloro‐2‐(hydroximino)‐1‐(4‐methyl‐2‐phenylthiazol‐5‐yl)ethanone and different reagents. Structures of the newly synthesized compounds were confirmed by elemental analysis and spectral data.     

Novel reduction of perfluoroalkyl ketones with lithium alkoxides

The reaction of tert-butyl N-(2-bromophenyl)carbamate (1) with ethyl perfluorooctanoate in the presence of tert-butyllithium did not give the desired N-(2-perfluorooctanoylphenyl)carbamate (3) but gave 1-hydroxy-1H-perfluorooctyl compound (4), which was supposed to be formed by the reduction of 3. A similar reaction of 2,2,2-trifluoroacetophenone with tert-butyllithium did not gave any reduction product. Detailed investigation showed that lithium ethoxide worked as the reducing agent of this abnormal reduction. By the reaction of lithium isopropoxide, an aldol product from 2,2,2-trifluoroacetophenone with acetone was isolated, while perfluoroheptyl or perfluoropropyl phenyl ketones were reduced by this alkoxide in a high yield without formation of the aldol adduct.     

Interaction of manganese(II), iron(II), cobalt(II), nickel(II), copper(II) and zinc(II) with acetylhydrazine, formed in situ; first crystal structure of tris(acetylhydrazine) nickel(II) perchlorate

A series of transition metal complexes of the type [M(ah)₃](ClO₄)₂ (1–6) [M = Mn^II, Fe^II, Co^II, Ni^II, Cu^II and Zn^II, ah = acetylhydrazine] have been prepared by the reaction of M(ClO₄)₂ · 6H₂O with acetylhydrazine formed in situ by the reaction of hydrazine hydrate and acetylsalicylic acid methyl ester. The chelating behaviour of acetylhydrazine and overall geometry of these complexes have been spectroscopically investigated by means of FT-IR, ¹H-n.m.r. and electronic spectral techniques, as well as by elemental analysis data, molar conductance values and magnetic susceptibility measurements. Single X-ray structure determination of complex (4) revealed three acetylhydrazine ligands coordinated to nickel ion in a bidentate manner maintaining an octahedral environment. In all other complexes too, an octahedral geometry has been proposed on the basis of results obtained by various physico-chemical studies.     

Modelling of three-dimensional mechanical systems using point coordinates with a recursive approach

In this paper, the dynamic simulation of constrained mechanical systems that are interconnected of rigid bodies is studied using projection recursive algorithm. The method uses the concepts of linear and angular momentums to generate the rigid body equations of motion in terms of the Cartesian coordinates of a dynamically equivalent constrained system of particles, without introducing any rotational coordinates and the corresponding rotational transformation matrix. Closed-chain system is transformed to open-chain by cutting suitable kinematical joints and introducing cut-joint constraints. For the resulting open-chain system, the equations of motion are generated recursively along the serial chains. An example is chosen to demonstrate the generality and simplicity of the developed formulation.     

Organophosphorus compounds: I. Simple,rapid, and reliable method for the simultaneous microdeterminaton of carbon,hydrogen, and phosphorus by the rapid straight empty tube method

A method for the simultaneous microdetermination of C, H, and P is presented. The organophosphorus compound is pyrolyzed in a 80-mm long silica sample capsule using the rapid straight empty tube method. Carbon and hydrogen are determined by conventional gravimetry. Oxides of phosphorus are quantitatively retained on the walls of the capsule. The P₅O₂, uptake is determined gravimetrically for the phosphorus determination.Organophosphorus compounds containing sulfur can also be analyzed following the same procedure. Electrolytic silver, heated at 550 °C, absorbs the oxides of sulfur. The results obtained fall within the acceptable limits of error.     

Unsteady hydromagnetic Couette flow of dusty fluid with temperature dependent viscosity and thermal conductivity

In the present paper the unsteady Couette flow and heat transfer of a dusty conducting fluid between two parallel plates with temperature dependent viscosity and thermal conductivity are studied. A constant pressure gradient and an external uniform magnetic field are applied. The governing coupled momentum and energy equations are solved numerically using finite differences. The effect of the variable viscosity and thermal conductivity of the fluid and the uniform magnetic field on the velocity and temperature fields for both the fluid and dust particles is discussed.     

Synthesis of some novel 3,7‐dimethyl‐4H‐pyrazolo[5,1‐c][1,2,4]triazin‐4‐ones

Some novel 3,7‐dimethyl‐6H‐pyrazolo[5,1‐c][1,2,4]triazin‐4‐ones were prepared (3a‐g) . Compounds 3a,b were treated with hydrazines to afford various products 7a,b, 8a,b, 9 and lla,b depending on the type of hydrazine derivative and reaction conditions. The benzoyloxyimino‐pyrazolo[5,1‐c][1,2,4]triazines (13a,b) were synthesized by refluxing of compounds 3a,b with hydroxylamine hydrochloride to afford the corresponding oxime derivatives followed by treatment with benzoyl chloride.     

The role of the cation in the oxygen isotopic exchange in crystalline sulfate salt hydrates

The oxygen isotopic exchange during dehydration and decomposition of five sulfate salt hydrates (CoSO₄·6H₂O, NiSO₄·7H₂O, ZnSO₄·7H₂O, CaSO₄·2H₂O, Li₂SO₄·H₂O) was studied in detail by temperature programmed desorption mass spectrometry (TPD-MS) in a supersonic molecular beam (SMB) inlet mode. Crystals of the ¹⁸O-enriched salts were grown and the detailed desorption steps of the various gaseous products released during dehydration and decomposition of these compounds were recorded. The desorption patterns confirmed the known characteristic stepwise dehydration of these salts, where regardless of the crystalline structure and composition, in all the salts (excluding the Li and Ca sulfates) a major group of n ? 1 loosely bounded water of crystallization molecules (out of total of n molecules in the fully hydrated form) are released at adjacent temperatures in a typical low temperature range (<200 °C), while the last, most strongly bounded water molecule, consistently desorbs at relatively higher temperatures (240 < T < 440 °C). Interestingly, it is established that the oxygen isotopic exchange occurs exclusively between that latter, most strongly bound water molecule, and the salt anion. Remarkably, the results point out that the exchange process is mostly of solid-solid nature. Finally, the results point out that the probability of the isotopic exchange increases with the increment in the desorption temperature of the last dehydration step, i.e. with the bond strength in the monohydrate, between the last water molecule of crystallization and the cation.     

Michael Addition of Activated Nitriles to 4[(+)-Camphor-10′-Sulfonylamino]acetophenone and Some of its Chalcones

4-[(+)-Camphor-10'-sulfonylamino]acetophenone ( 2 ) and some of its chalcones 3 were easily prepared in quantitative yields starting from (+)-camphor-10-sulfonyl chloride. Several new 2-oxo-, 2-thio-, as well as 2-amino-pyridines carrying the camphor sulfonylamino group as a substituent were synthesized easily in one step by Michael addition of several activated nitriles to compounds 2 and 3 . The synthesis of some fused pyridines also was investigated.