异硒氰酸酯参与合成2-亚胺基-1,3-硒唑-4-酮类化合物的研究

以异硒氰酸酯、苄胺、氯乙酰氯为原料,在三乙胺的作用下一锅法反应合成2-亚胺基-1,3-硒唑-4-酮衍生物,收率良好。其结构经1H NMR,13C NMR,IR和MS表征。     

Zur Fließfähigkeit von Schüttgütern – Definition und Meßverfahren

Flowability of Bulk Solids – Definition and Measuring Principles . The flowability of bulk solids has to be known for many practical applications. The present paper describes how the flowability is defined and on which physical properties it depends. Experimental determination of the flowability using a shear test is demonstrated. Conditions influencing measuremed results are described. Finally an overview of various methods used for characterization of the flowability of bulk solids is given.     

Zur Strukturaufklärung der Bromierungsprodukte von N-Aryl-2,4-dimethyl-buta-1,3-dien-sultamen-1,4

Structure Elucidation of Bromination Products of N-Aryl-2, 4-dimethyl-buta-1,3-diene-sultames-1, 4 The structure of bromination products of N-aryl-2, 4-dimethyl-buta-1, 3-diene-sultames-1, 4 1a–d , f is determined by 13-C-n.m.r. spectroscopy. As mono bromination product of N-phenylsultam 1a the 4-bromomethyl derivative 2a was isolated. Dibromination of sultames 1 yields 1-brom-4-brommethyl-sultames 3 and by tribromination 1,3-dibrom-4-brommethyl-sultames 4 are obtained.     

1H- und 13C -NMR-spektroskopische Untersuchungen an substituierten 1, 1-Dioxo-1, 2-thiazinen; Additivität der Substituenteneffekte

¹H- and ¹³C-N.M.R. Spectroscopic Investigations of Substituted 1, 1-Dioxo-1, 2-thiazines; Additivity of the Substituent Effects . The influence of various XCH₂ substituents (X: Cl, Br, I, SCN, SO₂CH₃, SC(NH₂)₂^⊕, Py^⊕) in the 3-, 5- and 3, 5-position of the 1, 1-dioxo-2-phenyl-1, 2-thiazine on the ¹H- and ¹³C-n.m.r. chemical shifts of the ring atoms is described. The substituent effects are additive. The ¹H- and ¹³C-n.m.r. chemical shifts of the 3, 5-substituted 1, 1-dioxo-1, 2-thiazines can be calculated from increments derived from the 3- and 5-substitued compounds.     

Zur Reduktion von 1,3-Thiaziniumsalzen; Synthese von 6,6′-Bi-1,3-thiazinylen und 6,6′-Bi-1,3-thiazinylidenen

On the Reduction of 1,3-Thiazinium Salts; Synthesis of 6,6′-Bi-1,3-Thiazinyls and 6,6′-Bi-1,3-Thiazinylidenes 1,3-Thiazinium perchlorates 1 are linked together in a reaction with zinc powder or at a cathode forming 6,6′-bi-1,3-thiazinyls 3 . This reaction proceeds via radical intermediates 2 . Evidence of the existence of the very short-lived radicals is given by means of ring-disk-voltammogrammes as well as by electrochemical luminescence excitation. The 6,6′-bi-1,3-thiazinyls 3 undergo the reverse fission at a platinum anode resulting in thiazinium salts 1 , whereas the dehydrogenation by chloranile yields the violet 6,6′-bi-1,3-thiazinylidenes 6 .     

Die Leistungsfähigkeit von Winterrapssorten mit 00-Qualität

Performance of Winter Rape Seed Varieties with Double Quality After realization of the first quality characteristic — exemption of erucic acid — of rape seed in 1974, rape seed cultivators work at the second quality characteristic, the exemption of glucosinolates. The attempts resulted 1981 in the introduction of the first winter rape seed variety with double quality LIBRADOR in the German list of varieties. Already one year later — 1982 – the variety LIGLANDOR followed, and 1983 the varieties LINDORA, LIROPA and ELENA were taken up in the list. The difference in the performance between the 0-varieties and the 00-varieties decreases with every new variety introduction. The difficulty of testing the performance, caused by animal feed, led to the fact that the spread of the results between the 00-varieties is essentially higher than between the 0-varieties.     

Synthese von Dibenzo-tetrathiafulvalenen mit 1,3-Dithiol-2-yl-phosphonsäureester-Struktur

Synthesis of Dibenzo-tetrathiafulvalenes Containing 1,3-Dithiol-2-yl-phosphonic Ester Structures 1,3-Dithiol-2-ylphosphonate esters ( 3a-d ) with a dibenzo-tetrathiafulvalene unit were synthesized directly from trialkylphosphite and 6,6′-dioxo- ( 2a , c ) and 6,6′-dithioxo-4,4′,8,8′-tetrakis(alkylthio)-2,2′-bi-1,3,5,7-tetrathia-s-indacenylidenes ( 2b , d ). The influence of the type of trialkylphosphite, of the reaction temperature and the solvent on the regioselectivity of the reaction was studied. In toluene the tristetrathiafulvalene ( 4c ) was exclusively obtained from 2c .     

Struktur und elektrische Leitfähigkeit von polymeren organischen Halbleitern

In this review article we want to give information about low molecular and polymer organic semiconductors, which were recently synthesized in our institute. Specific electric conductivities up to σ_298°K = 9.0 · 10^?5Ω^?1 · cm^?1 and thermic activation energies of E = 0.30 eV of polyenearylenes, respectively -heteroarylenes were measured. Polyazomethines have a maximum σ_298°K = 3.3 · 10^?9Ω^?1 · cm^?1 and E = 0.35 eV. Polymers with indophenine units have conductivities up to σ_298°K = 1.1 · 10^?4Ω^?1 · cm^?1 and E = 0.39 eV. A maximum of σ_298°K = 5.0 · 10^?2Ω^?1 · cm^?1 and E = 0.05 eV was found for bis-(1.2-dicyanoethylenedithiolo)-metal salts. Polymers with a phthalocyanine- or hemiporphyrazine-like structure achieve a conductivity of σ_298°K = 2.3 · 10^?2Ω^?1 · cm^?1 and E = 0.15eV. Coordination polymers of dimercaptomaleic acid, respectively their monoamide show a maximum of σ_298°K = 3.2 · l0^?lΩ^?l · cm^?1 and E = 0.20 ev. Polymers with σ_298°K ≤1.5 · 10^?5 Ω^?l · cm^?l and E ≥ 0.5 eV were obtained by the polymerization of succinonitrile. All the investigated substances show an electronic conductivity. The existence of an ionic conductivity could, in all cases, be excluded by using direct current measurements over a long period of time.     

Zur Analyse von Milchsäure-Glykolsäure-Copolyestern

Für L-(–)-Lactid-Glykolid-Copolyester (3) wurden drei voneinander unabhängige Analysenmethoden zur Bestimmung der Copolymeren-Zusammensetzung ausgearbeitet. Die ¹H-NMR-Spektroskopie wurde für Copolyester mit Lactid-Gehalten über 10 Gew.-% erfolgreich angewandt, nachdem mit Trifluoressigsäure ein geeignetes Lösungsmittel gefunden war. Insbesondere für die praktisch interessanten Materialien mit kleinem Lactid-Anteil, wie z. B. resorbierbares chirurgisches Nahtmaterial, eignen sich die Messung der optischen Rotation sowie eine chemische Methode, die auf der quantitativen Bestimmung der Milchsäure nach vorhergehender alkalischer Totalhydrolyse beruht.     

Zur Herstellung von 1,3,4- Oxadiazol-2-carbonsäurederivaten

Preparation of 1,3,4,-Oxadiazol-2-carboxylic Acid Derivatives The synthesis of 5-substituted-1,2,4-oxadiazol-2-carboxylic acid derivatives 3a-g and 4a-g by cyclodehydratation of diacylhydrazines 1a-g and 2a-g are described. Further derivatives 6 to 9 are obtained from 1,3,4-oxadiazol-2-carboxethyl esters 3 .     

Der Einfluß von Anion- und Kationtensiden auf die chemische Reaktionsfähigkeit von Wolle

Influence of Anionic and Cationic Surfactants on the Chemical Reactivity of Wool The alkaline degradation of cystine in wool is diminished by anionic detergents and increased by cationic detergents. The reaction with sulphite is influenced in a similar manner. In acidic media, the opposite effect is exerted by ionic detergents on the acid hydrolysis of wool peptide bonds; hydrolysis is enhanced by anionic detergents and diminished by cationics. Nonionic detergents are without any effect on the chemical reactivity of wool. The results are explained in terms of changes in electrical charges on the fibre surface, due to adsorption of detergent ions.