Search results for "Mass spectrum"
showing 10 items of 302 documents
ChemInform Abstract: Preparation and Structural Characterization of (Me3SiNSN)2Se, a New Synthon for Sulfur-Selenium Nitrides.
2010
The reaction of (Me(3)SiN)(2)S with SeCl(2) (2:1 ratio) in CH(2)Cl(2) at -70 degrees C provides a route to the novel mixed selenium-sulfur-nitrogen compound (Me(3)SiNSN)(2)Se (1). Crystals of 1 are monoclinic and belong the space group P2(1)/c, with a = 7.236(1) A, b = 19.260(4) A, c = 11.436(2) A, beta = 92.05(3) degrees, V = 1592.7(5) A(3), Z = 4, and T = -155(2) degrees C. The NSNSeNSN chain in 1 consists of Se-N single bonds (1.844(3) A) and S=N double bonds (1.521(3)-1.548(3) A) with syn and anti geometry at the N=S=N units. The N-Se-N bond angle is 91.8(1) degrees. The EI mass spectrum shows a molecular ion with good agreement between the observed and calculated isotopic distributions…
Pyrrole Studies XXVII.1Utilisation of 1-Methyl-2-pyrrolyl Lithium in the Synthesis of 1-Methyl-2-substituted Pyrroles
1982
Abstract Although metallation of 1-substituted pyrroles with alkyl lithium reagents to give the lithiated derivatives has been recorded by several research groups,4–6 only limited use has been made of these derivatives in the synthesis of 1,2-disubstituted pyrroles. Subsequent to ourinitial studies,7 it was reported that tetrahydrofuran was the solvent of choice for the formation of the mono-lithiated pyrrole derivative and that the rate of the metallation was accelerated by the presence of TMEDA.6 We had noted,7 however, that prolonged reaction of n-butyl lithium with 1-methylpyrrole in a 2:1 mixture of tetrahydrofuran:hexaneat ca 18°C in the absence of TMEDA gave 1-methyl-2-pyrrolyl lithi…
High-Yield Synthesis of 20-, 24-, and 28-Membered Macropentolide, -hexolide, and -heptolide, Respectively, from (R)- or (S)-3-hydroxybutanoic acid un…
1988
The macrocyclic pentolide 1, hexolide 2, and heptolide 3 constitute ca. 80% of the oligomers formed in ca. 50% yield from enantiomerically pure 3-hydroxybutanoic acid under Yamaguchi's macrolactonization conditions. The FAB mass spectra of the MH+, M Na+, and MCs+ are reported (Figs. 2, 3, 5, and 6). No cyclic tetramer is detected. The 1H-NMR spectra of the cyclic oligomers, of the monomer, and of the polymer (PHB) are very similar (Fig. 4). Directed synthesis of the open-chain dimer and tetramer of 3-hydroxybutanoic acid and attempted cyclization do not lead to the isolation of the cyclic tetramer.
Muskelrelaxantien, 4. Mitt. Monoacylbutyroguanamine
1986
Die Umsetzung von Butyroguanamin (1) mit den Carbonsaureanhydriden 2a−f bei 80–120° fuhrt zu den Monoacylbutyroguanaminen 3a−f, deren Struktur durch IR-, 1H-NMR- und MS-Spektren untermauert wird. Unter den hier beschriebenen Verbindungen weisen insbesondere 3e muskelrelaxierende und antidiabetische und 3a trichomonazide und antivirale Wirksamkeit auf, wahrend mit 3b−d herbizide Wirkungen beobachtet werden. Muscle Relaxants, IV: Monoacylbutyroguanamines Reaction of butyroguanamine (1) with the carboxylic acid anhydrides 2a−f at 80–120°C leads to the monoacylbutyroguanamines 3a−f, the structure of which is supported by IR, 1H-NMR, and mass spectra. Among the compounds described here, particul…
Synthesis of polycyclic fused benzimidazole derivatives
1977
Am easy method for the synthesis of tetraeyclie systems containing an imidazole and an iso-thiazole or an imidazole and a thiazine ring, by reacting 2H-1,3-benzothiazine-2-thion-4(3H)one with aromatic primary diarnines is reported. The structures were assigned based upon mass spectra and modes of cleavage of the compounds. The most important fragments are described.
Field Desorption Mass Spectra of Gastrine Peptides and Glutathione Derivatives
1979
Oligopeptides comprising the sequence of the C-terminal tetrapeptide of gastrine, Trp-Met-Asp-Phe-NH2, and several derivatives of glutathione, γ-Glu-Cys(SR)-Gly, were characterized by field desorption mass spectrometry. The field desorption mass spectra obtained at various field ion emitter temperatures reveal abundant molecular ions and fragmentation reactions that yield partial sequence information. In the series of glutathione derivatives investigated, characteristic ions formed by cleavage of the γ-Glu-Cys peptide bond determine the substituent at the Cys residue and can therefore be used to identify corresponding conjugation products of drug metabolites with glutathione.
Stufenweise darstellung eines cycloheptamers aus p-kresol, 4-tert-butylphenol und formaldehyd. Vergleich mit einem phenolischen, heptanuklearen kette…
1980
A phenolic cycloheptamer (11) and an analogous chain oligomer (10) with nearly the same structure were gained by stepwise syntheses. The cycloheptamer has a higher melting point and a better solubility in chloroform. In contrast to the chain oligomer his infrared spectrum indicates a stronger association of the hydroxyl groups which is not influenced by the solvent. The mass spectra announce a preferred statistical cleavage along the chain of compound 10 and a great stability of the ring of 11 which preferentially loses his substituents. The 1H NMR spectra confirm the constitutions of the chain (10) and ring compound (11). The cycloheptamer is distinguished by a ring inversion or a pseudoro…
Darstellung und charakterisierung von einigen neuen bis(1-phenylvinyl)-verbindungen
1974
Einige neue Bis(1-phenylvinyl)-Verbindungen (1b, c und 2a–d) wurden aus den entsprechenden Diacetylverbindungen und Phenylmagnesiumbromid dargestellt. Ihre IR-, NMR-und Massenspektren werden diskutiert. Some new bis(1-phenylvinyl) compounds (1b, c and 2a–d) were prepared from the corresponding diacetyl compounds and phenyl magnesium bromide. Their IR, NMR and mass spectra are discussed.
A resorcinol derived calix[5]arene with C5-symmetry
1994
Abstract Condensation of 2,4-dihydroxy-3-hydroxymethyl benzophenone (4) in dioxane/H2SO4 gave the cyclic pentamer 5, a calix[5]arene with regular incorporation of the resorcinol units via their 2- and 6-positions. The structure follows from the 1H NMR and mass spectra and was further confirmed by single crystal X-ray analysis. Dynamic NMR in C2D2Cl4 gave a surprisingly high barrier of ΔG‡ = 17.3 kcal/mol for the cone-to-cone ring inversion.
ChemInform Abstract: Alkaloid Determination in Crude Extracts from Cortex Quebracho and Opium Applying Capillary Electrophoresis and Capillary Electr…
2010
The applicability of capillary electrophoresis with UV and electrospray ionisation (ESI)-mass spectrometric detection to the determination of alkaloids in crude extracts of Cortex Quebracho and opium has been investigated. The use of a buffer electrolyte consisting of aqueous ammonium acetate (pH 3.1) and acetonitrile resulted in a high performance of peak resolution. Most of the alkaloids have been identified according to the signal of the protonated molecular ion in the ESI mass spectrum