Purification of 3-ethoxycarbonylquinuclidine and its conversion to 3-quinuclidinecarboxylic acid and 3-quinuclidinylmethanol

3-Ethoxycarbonylquinuclidine obtained by the Grob method is a mixture of 3-ethoxycarbonyl-1-azabicylo-[2.2.2]- and, according to ¹³C NMR data, 5-ethoxycarbonyl-5-azatricyclo[3.2.1.0^2,7]octanes (1621). 3-Ethoxy-carbonylquinuclidine was purified by recrystallization of the hydrochloride, hydrolyzed by water to 3-quinuclidinecarboxylic acid, and reduced by LiAlH₄ to 3-quinuclidinylmethanol.Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 11, 1509–1512, November, 1992.     

The Use of tert-Butyl Vinyl Ether in Stepwise Electrophilic Addition Reactions

tert-Butyl vinyl ether (1) reacts with p-TolSCl to give 2-tert-butoxy-2-chloroethyl p-tolyl sulfide (2). In the presence of SnCl₄, 2 reacts with silyl enol ethers, allyltrimethylsilane, and vinyl ethers to form a C-C bond. In the case of vinyl ethers, the reaction proceeds through the formation of the 5-membered sulfonium salt intermediate which in turn can react with H₂O, TMSCN, allyltrimethylsilane, and Grignard reagents.     

Evaluation of the ion drift parameters in dielectric films from the dynamic current-voltage characteristics

The nonequilibrium dynamic current-voltage characteristics of the MDM structure are analyzed on the basis of the exact numerical solution of the electrical transport equations with consideration of the drift and diffusion of the charge carriers in an electrically neutral dielectric with blocking electrodes. A new method is proposed for the evaluation of the charge carrier mobility from the position of the current maximum on the dynamic current-voltage characteristic curves. The role of the diffusion component of the current is evaluated.Translated from Izvestiya Vysshikh Uchebnykh Zavedenii, Fizika, No. 1, pp. 87–94, January, 1984.     

A one-pot synthesis of beta-C-glucopyranosides from exo-glucal,p-tolylsulfenyl chloride,an alpha-methoxyalkene,and an external nucleophile

[formula: see text] beta-C-Glycosides were synthesized in one-pot experiments using the following sequence of four reactions: (i) addition of p-TolSCl to an alpha-methoxyalkene, (ii) generation of the episulfonium ion from a beta-(arylsulfanyl)alkyl chloride, (iii) reaction of the episulfonium intermediate with benzylated exo-D-glucal to form a cyclic five-membered sulfonium salt, and (iv) quenching of the sulfonium salt with the external nucleophile: H2O, CH3OH, or NaCNBH3.     

The analysis of the electret-depolarization based on various models

This paper gives an analysis of the process of depolarization of an electret, based on models which allow for volume charges of both signs which have been injected into the dielectric and held in traps. It is shown that an inversion of the direction of the discharge current can be observed during electret depolarization.Translated from Izvestiya Vysshikh Uchebnykh Zavedenii, Fizika, No. 6, pp. 104–110, June, 1974.     

A TEM and XRD study of the SbNbSe3 misfit layer structures

Two new misfit layer structures have been synthesized within the Sb-Nb-Se system. Powder X-ray diffraction and electron microscopy techniques (electron diffraction, HREM, XEDS) have been used to determine the nature of their structure. According to TEM and XEDS data (for more than 15 crystals studied) both phases are monolayer type, i.e. (SbSe)1+delta (NbSe2). Electron microscopy reveals a composite modulated structure that consists of the periodical intergrowth of a pseudotetragonal SbSe layer, denominated as Q, and a pseudohexagonal layer NbSe2, denominated as H. Both layers fit along b, stack along c and do not fit along a (misfit) giving rise to an incommensurate modulation along this direction. The two phases differ in the symmetry of the Q layers being in one case orthorhombic (for delta = 0.17) and monoclinic in the other (for delta = 0.19). After the characterization of the sample by electron microscopy the unit cells of the basic layers could be refined for both phases by powder X-ray diffraction: aQ = 5.824(2) A, bQ = 5.962(5) A, cQ = 23.927(6) A, alpha = 90 degrees, beta = 90 degrees and gamma = 90 degrees and aH = 3.415(5) A, bH = 5.962(6) A,, cH = 11.962(1) A, alpha = 90 degrees, beta = 90 degrees and gamma = 90 degrees for the orthorhombic phase; aQ = 5.844(2) A, bQ = 5.981(1) A, cQ = 23.919(5) A, alpha = 90 degrees, beta = 90 degrees and gamma = 96.00(3)degrees and aH = 3.439(1) A, bH = 5.994(2) A, cH = 11.956(3) A, alpha = 90 degrees, beta = 90 degrees and gamma = 90 degrees for the monoclinic phase. The phase with the monoclinic Q-sublattice often appears as twinned crystals. The more abundant crystals are disordered intergrowths of both monolayer phases.     

Gas formation in liquid hydrocarbon dielectrics under the action of particle discharges

A study is performed of destruction of the hydrocarbon liquid n-nonane under the action of particle discharges in a test cell with needle-plane electrode system. The process of gas formation is studied, and the products of electrical aging are identified.Translated from Izvestiya Vysshikh Uchebnykh Zavedenii, Fizika, No. 4, pp. 24–27, April, 1986.     

Condensation of N-ethylpiperid-4-one with benzaldehyde

Reaction of N-ethylpiperid-4-one with benzaldehyde and KOH in 65% aqueous methanol gives 2,7-diethyl-10a-hydroxy-9-phenyl-4-(phenylmethylene)-2,7-diaza-10-oxa-1,2,3,4,5,6,7,8,8a, 10a-decahydroanthracene. In the presence of HCl/EtOH, 3,5-bis(phenylmethylene)-1-ethylpiperid-4-one is formed. In the presence of HCl/AcOH, 2,7-diethyl-9-phenyl-4,5-bis(phenylmethylene)-2,7-diaza-10-oxa-1,2,3,4,5,6,7,8-octahydroanthracene is formed.Center for the Chemistry of Medicinal Agents, All-Russian Chemicopharmaceutical Institute, Moscow 119815. Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 9, pp. 1247–1249, September, 1998.