Zur reaktionsweise von triafulvenen mit azomethinyliden

The reaction of the azomethine ylides 2a–c with cyclopropenones 3 and of 2a with methylene cyclopropenes 7 leads via (3+3)-cycloaddition to pyridones-4 5 and 1,4 - dihydro - N - methyl - 4 - methylene - pyridines 8, respectively. The merocyanine systems 8 exhibit marked solvatochromic and thermochromic properties.     

Synthesen von Heterocyclen, 130. Mitt.: Über das Glomerin und das Arborin

Zusammenfassung Es werden einstufige Synthesen desGlomerins (2) [1,2-Dimethyl-4(1H)-chinazolinon] und desArborins (3) [1-Methyl-2-benzyl-4(1H)-chinazolinon] bekanntgegeben.

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Syntheses of heterocycles, CXXX: Glomerine and arborine

A one step synthesis ofglomerine (2) [1.2-dimethyl-4(1H)-quinazolinone] andarborine (3) [1-methyl-2-benzyl-4(1H)-quinazolinone] is described.

     

Analytical applications of crown ethers : III. Extraction and determination of nitrophenol isomers

The oxidation of aldehydes by dicyclohexyl-18-crown-6-potassium permangante complex is presented. Results obtained by this procedure showed that the presence of crown ether (DCC) and the catalyst play an important role in the oxidation of the aldehydes. The stoichiometry found corresponds to 2 μeq of permanganate per 1 μmol of aldehydes in all cases. Alcohols and ketones are not oxidized. Finally, a method for quantitative evaluation of aldehydes is proposed.     

Untersuchungen zur Temperaturabhängigkeit charakteristischer IR-Absorptionen, 9. Mitt.: Zur Tautomerie des “o-Hydroxymandelsäurelactons”

Zusammenfassung Die Abhängigkeit der Struktur des o-Hydroxymandelsäurelactons von Lösungsmittel und Temperatur wird mit Hilfe IR- und NMR-spektroskopischer Methoden nachgewiesen.

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The temperature and solvent dependence of the structures of 2-hydroxymandelic acid lactone and dioxindole have been shown by IR and NMR spectroscopy.

     

Metallkomplexe mit anionischen Liganden von Elementen der 4. Hauptgruppe. VIII. Pentacarbonyl-trihalogenstannido-metallat(O)-Komplexe von chrom,molybdän und wolfram mit fluor- und jodhaltigen stannidliganden

Metal Complexes with Anionic Ligands of Elements of the Main Group IV. VIII Pentacarbonyltrihalogenostannidometalate(O) Complexes of Chromium, Molybdenum, and Tungsten with Fluorine and Iodine Containing Trihalogenostannido Ligands In methylenechloride [As(C₆H₅)₄][SnF₃] readily reacts with the metalhexacarbonyls forming the arsoniumsalts of the pentacarbonyltrifluorostannidometalate(O) complexes, [M(CO)₅SnF₃]^? (M ? Cr, Mo, W). Exclusively by the reaction of the intermediately formed complex Cr(CO)₅THF only one pure triiodostannidometalate(O) Complex, [N(C₂H₅)₄][Cr(CO)₅SnJ₃], could be isolated. The trihalogenostannidometalate(O) complexes [M(CO)₅SnClX₂]^? (X ? F: M ? Cr, Mo, W; X ? J: M ? Cr) could be prepared by SnX₂-insertion reactions of the [M(CO)₅Cl]^? complexes. The bonding properties of the halogenostannide ions are discussed on the bases of the IR spectra of their metalate(O) complexes.     

CeAgAs2 — a New Derivative of the HfCuSi2 Type of Structure: Synthesis,Crystal Structure and Magnetic Properties

Single crystals of CeAgAs₂ have been obtained by chemical transport reactions starting from a pre‐reacted powder sample. The crystal structure was solved using X‐ray diffraction (space group Pmca, No. 57, a = 5.7586(4) Å, b = 5.7852(4) Å, c = 21.066(3) Å, Z = 8) and refined to a residual of R(F) = 0.029 for 46 refined parameters and 1020 reflections. The structure of CeAgAs₂ represents a new distorted and ordered variant of the HfCuSi₂ type. The characteristic feature of this structure are infinite cis‐trans chains of As atoms with As—As distances of 2.563(1) Å and 2.601(1) Å. CeAgAs₂ is paramagnetic (μ_eff = 2.37 μ_B, θ = —10.5(2) K), with antiferromagnetic ordering at 5.5(2) K and exhibits a metamagnetic transition starting at 4.6 kOe and T = 1.8 K.     

Comprehensive gas chromatography of high-boiling halogenated compounds

Summary Comprehensive gas chromatography is an excellent technique for separating complex mixtures. If, however high-boiling compounds such as polychlorinated biphenyls have to be analysed, proper adjustiment of the temperature of the modulator turns out to be very important in maintaining the performance of the system. It is shown that miniaturisation of the column-to-modulator coupling, adequate selection of the modulating conditions and, for halogenated compound mixtures, the use of a micro electron-capture detector, can solve experimental problems previously encountered with high boilers.     

Derivatization of carboxylic acids with 9-bromomethylacridine using micellar phase-transfer catalysis

Summary Micellar phase-transfer catalysis (MPTC) offers the opportunity to derivatize carboxylic acids directly in an aqueous matrix without prior extraction of the acids into a suitable aprotic solvent. The currently developed MPTC system consists of a non-ionic surfactant, Arkopal N-130, an ion-pair agent, tetrakis-(decyl)-ammonium bromide, and a novel fluorescence reagent, 9-bromomethylacridine. The MPTC system can be applied to the derivatization of many types of carboxylic acids. The reaction rate is affected by the lipophilicity of the acid and by the presence of other functional groups. For lipophilic carboxylic acids the reaction is complete within 5 min at 60°C and pH 7.0.     

Vibrational spectra of compounds Ln2MoO6 and Ln2WO6

The vibrational spectra of compounds Ln₂WO₆ and Ln₂MoO₆ (Ln = lanthanide, including Y and Bi) are reported. Neglecting details it is possible to assign the internal vibrations of the molybdate and tungstate group. The results are in agreement with the structural data known up till now and suggest further that tungsten in the unknown Y₂WO₆ structure is in six-coordination, that Bi₂MoO₆ shows still another modification than koechlinite and that vibrational spectroscopy may yield additional structural information for compounds like those under consideration.     

Bis(trifluoroacetoxy)iodobenzene,a new oxidant in potentiometric titrations

A new oxidimetric titrant, bis(trifluoroacetoxy)iodobenzene is proposed for potentiometric titrations in acetonitrile and water-acetonitrile media. The general analytical conditions for using this titrant and the results for the potentiometric titrations of various inorganic and organic reductants are described.