New method of synthesis 1-halogermatranes,germatranyl esters of H-O acids,and their stereoelectronic structure

A fundamentally new method for the synthesis of 1-halogermatranes and germatranyl esters of oxygen-containing acids has been developed. Using this method germatranes XGe(OCH₂CH₂)₃N (X = Hal, ClO₄)were synthesized, their elemental analysis was determined, and their stereoelectronic structure was studied by the methods of multinuclear NMR, mass spectrometry, and IR spectroscopy. The obtained data correlate with the results of quantum chemical calculations.     

Mass spectra of new heterocycles: XII. Main fragmentation pathways of the molecular ions of 5-methylsulfanyl-1-vinyl-1H-pyrrol-2-amines under electron impact and chemical ionization

Fragmentation patterns of 5-methylsulfanyl-1-vinyl-1H-pyrrol-2-amines under electron impact (70 eV) and chemical ionization (methane as reactant gas) were studied for the first time. The electron impact mass spectra of all the examined compounds contained a strong peak of molecular ion which decomposed along four pathways. Two pathways involved cleavage of the C-S bonds with elimination of methyl (major) and MeS radicals (minor), and the two others, decomposition of the pyrrole ring. The chemical ionization mass spectra displayed strong molecular, [M + H]⁺, and odd-electron [M + H ? SMe]⁺ ion peaks. N,N-Dimethyl-5-methylsulfanyl-4-phenyl-1-vinyl-1H-pyrrol-2-amine under chemical ionization with methane as reactant gas characteristically decomposed with formation of [M ? C₄H₉N]⁺ as the only fragment ion.     

1,1-Diethynylsilacycloalkanes and Propellanes Based Thereon

Previously unknown 1,1-diethylnylsilacycloalkanes (CH₂)4nSi(C& = CH)₂ (n = 3, 4) were prepared by the reaction of HC& = CMgBr with 1,1-dichlorosilacycloalkanes (CH₂)4nSiCl₂ (n = 3, 4). The reaction of (CH₂)₄Si(C& = CMgBr)₂ with (CH2)4SiCl2 in THF under conditions of high dilution gives cyclo(tetramethylene)- silethynes [(CH2)4SiC& = C]4 with an admixture of cyclodi(tetramethylene)silethyne [(CH2)4SiC& = C]2. The re- action of Me2Si(C& = CSiMe2C& = CMgBr)2 with (CH2)4SiCl2 was used to prepare 1,1,4,4,7,7-hexamethyl-10,10- tetramethylene-1,4,4,10-tetrasilacyclododeca-2,5,8,11-tetrayne.     

Chlorination of secondary phosphine selenides with the system CCl4/NEt3

Russian Journal of General Chemistry -     

Optimization of the synthesis of 2-phenyl-1,2,3-triazole

The synthesis of 2-phenyl-1,2,3-triazole by the cyclization of glyoxal phenylosazone in high-boiling solvents in the presence of copper triflate catalyst has been optimized. The structure of the product was confirmed by data of IR, ¹H, ¹³C, and ¹⁵N NMR spectroscopy, mass spectrometry, and elemental analysis.     

Radical addition of secondary phosphine sulfides and selenides to vinyl tellurides

The regiospecific addition of secondary phosphine sulfide and phosphine selenide to alkyl vinyl tellurides proceeds under radical initiation (AIBN, 65–70 °C, 2.5–3.5 h) to afford the anti-Markovnikov adducts, (2-alkyltellanylethyl)phosphine chalcogenides, in 86–99% yields.     

Synthesis and reductive splitting of tellurium-containing oligomers on the basis of 1-bromo-2-methyl-3-chloropropane

The results of the synthesis of tellurium-containing oligomers based on 1-bromo-2-methyl-3-chloropropane are presented. By the example of the reductive splitting of tellurocol the possibility is demonstrated of the synthesis of methyltellanyl derivatives, which are valuable reagents for organic synthesis and for the design of coordination compounds.