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  • 1
    ISSN: 1432-1904
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Chemistry and Pharmacology , Natural Sciences in General
    Type of Medium: Electronic Resource
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  • 2
    ISSN: 1432-1904
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Chemistry and Pharmacology , Natural Sciences in General
    Type of Medium: Electronic Resource
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  • 3
    ISSN: 1042-7163
    Keywords: Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A series of phosphoranes with pentacovalent phosphorus contained in a 1,3,2-dioxaphosphorinane ring have been studied by 1H NMR. One compound was investigated by low-temperature 13C NMR and another by X-ray crystallography. Although the 1H NMR parameters observed are time-averaged, the coupling constants can be accounted for if the phosphoranes have the six-membered ring attached apical-equatorial to phosphorus and occupy in solution rapidly isomerizing boat or slightly twisted boat conformations similar to that found in the X-ray study.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
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  • 4
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 561 (1988), S. 49-56 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Oxidative Addition of Hexafluoroacetone at 1-Chloro-, 1-(2,2,2-Trifluoroethoxy)- and 1-[2,2,2-Trifluoro-1-(trifluoromethyl)ethoxy]phosphorinaneHexafluoroacetone adds oxidatively to 1-chlorophosphorinane (1) forming the 1,3,4λ5σ5-dioxaphospholane 2 which reacts with antimony pentachloride to give the phosphonium salt 3 showing a ring rearrangement. The hydrolysis of 2 furnishes the phosphinate 4 under splitting off hexafluoroacetone. Following a different reaction pathway 1 and hexafluoroacetone yield also 1-chloro-1-oxo-λ5σ4-phosphorinane (5a) and 1-chloro-1-[2,2,2-trifluoro-1-(trifluoromethyl)ethylidene]-λ5σ4-phosphorinane (6). From the phosphinites 7 and 8 the 1,2λ5σ5-oxaphosphetanes 9, 10a and 10b are obtained, in which the four membered ring is annellated at the phosphorinane ring. Substituent permutation processes are not observed in 9, 10a and 10b.
    Notes: Hexafluoraceton addiert sich oxidativ an 1-Chlorphosphorinan (1) zu dem 1,3,4λ5σ5-Dioxaphospholan 2, das mit Antimonpentachlorid unter Ringumlagerung das Phosphoniumsalz 3 ergibt. Die Hydrolyse von 2 liefert das Phosphinat 4, wobei Hexafluoraceton abgespalten wird. Auf einem anderen Reaktionsweg bildet sich aus 1 und Hexafluoraceton auch 1-Chlor-1-oxo-λ5σ4-phosphorinan (5a) sowie 1-Chlor-1-[2,2,2-trifluor-1-(trifluormethyl)-ethyliden]-λ5σ-phosphorinan (6). Die Phosphinite 7 und 8 setzen sich zu 1,2λ5σ5-oxaphosphetanen 9, 10a und 10b um, in denen der Vierring an den Phosphorinanring anelliert ist. Substituenten-Umordnungsprozesse sind an 9, 10a und 10b nicht zu beobachten.
    Additional Material: 1 Tab.
    Type of Medium: Electronic Resource
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  • 5
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 386 (1971), S. 297-315 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Pentacarbonyl iron and tricarbonyl nitrosyl cobalt have been found to react with CF2Br2, CF2Br · CF2Br and CF2: CBr2 on UV irradiation to yield (CO)3Fe(CF2)2 (CO)Fe(CO)3 (I), (CO)3Co(CF2)2Co(CO)3 (II), BrC2F4Fe(CO)4Br (III), BrC2F4Co(CO)4 (IV), C2F2Br2Fe(CO)4 (V) and C4F4Br2Fe(CO)4 (VI). The structures of the new compounds are discussed on the basis of their mass and IR spectra.
    Notes: Durch UV-Bestrahlung der Dämpfe von Fe(CO)5 und CF2Br2 bzw. der Lösung von Co(CO)3NO in CF2Br2 konnten m̈-Carbonyl-di-m̈-difluormethylen-bis(tricarbonyleisen) (I) und Di-m̈-difluormethylen-bis(tricarbonylkobalt) (II) dargestellt werden. Die Bestrahlung des Dampfgemisches von Fe(CO)5 und CF2BrCF2Br und der Lösung des Carbonyls in dem Fluorbromäthan ergab β-Brom-tetrafluoräthyl-tetracarbonyleisenbromid (III), der Lösung von Co(CO)3NO in CF2BrCF2Br β-Bromtetrafluoräthyl-tetracarbonylkobalt (IV). (III) entstand auch bei der Bestrahlung einer Lösung von Fe(CO)5 in CF2Br2. Durch Photolyse der Dämpfe von Fe(CO)5 und CF2CBr2 sowie der Lösung des Carbonyls in dem Olefin entstanden 1,1-Dibrom-2,2-difluoräthylen-tetracarbonyleisen (V) und 2,3-Dibrom-tetrafluorbuten(2)-tetracarbonyleisen (VI). Die Strukturen der neuen Verbindungen werden auf der Grundlage ihrer Massen- und IR-Spektren diskutiert.
    Additional Material: 7 Tab.
    Type of Medium: Electronic Resource
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  • 6
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 507 (1983), S. 93-99 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Reactions of a Tetraalkoxy HydrospirophosphoraneThe hydrophosphorane HP[OC(CF3)2C(CF3)2O]2 is oxidized by dimethylsulfoxide to form a hydroxy phosphorane, which may be silylated easily. Chlorine and bromine react to give the corresponding halo spirophosphoranes. FP[OC(CF3)2C(CF3)2O]2 is obtained from FPCl2[OC(CF3)2C (CF3)2O] and Li2[OC(CF3)2C(CF3)2O]. In the presence of triethyl amine HP[OC(CF3)2C(CF3)2O]2 is converted by benzylbromide or acetylchloride to RP[OC(CF3)2C(CF3)2O]2 (R = PhCH2, MeC(O)). Trimethylphosphine performs an acid-base reaction producing a thermally unstable Me3PH+{P[OC(CF3)2C(CF3)2O]2}-. The hydrolysis of the parent compound gives phosphorous acid and perfluoropinacole.
    Notes: Das Hydrophosphoran HP[OC(CF3)2C(CF3)2O]2 wird durch Dimethylsulfoxid zu einem Hydroxyphosphoran oxidiert, welches leicht silyliert werden kann. Chlor und Brom ergeben die entsprechenden Halogenspirophosphorane; FP[OC(CF3)2C(CF3)2O]2 wird aus FCl2P[OC(CF3)2 C(CF3)2O] und Li2[OC(CF3)2C(CF3)2O] erhalten. In Gegenwart von Triethylamin reagiert HP[OC(CF3)2C(CF3)2O]2 mit Benzylbromid bzw. Acetylchlorid zu RP[OC(CF3)2C(CF3)2O]2 (R = PhCH2, MeC(O)). Trimethylphosphin setzt sich in einer Säure-Base-Reaktion um zu dem thermisch instabilen Me3PH+{P[OC(CF3)2C(CF3)2O]2}-. Die Hydrolyse der Stammverbindung ergibt phosphorige Säure und Perfluorpinakol.
    Additional Material: 1 Tab.
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  • 7
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Chemistry of Phosphorus Fluorides. XL. Phosphazenes of the Type RF2P=N—PF2 and their Tetracarbonvlmolybdenum ComplexesReaction of Fluorophosphorances, RPF4 (R = F, Ph), with bis(trimethylsilyl)-aminodifluorophosphine, (Me3Si)2N · PF2, gives rise to cleavage of the Si-N bond in the latter and phosphazenes of the type, RF2P=N—PF2, are formed. Displacement of the coordinated cycloolefin with formation of cis-(RF2P=N—PF2)2Mo(CO)4 occurs upon reaction of C7H8Mo(CO)4 (C7H8 = bicycloheptadiene) with RF2P=N—PF2. A complex, cis-[(Me3Si)2N · PF2]2Mo(CO)4 has also been obtained. Characterization of the compounds was by i.r., mass, 19F, and 31P n.m.r. spectroscopy.
    Notes: Durch Reaktion von Fluorphosphoranen RPF4 (R = F, C6H5) mit Bis(trimethylsilyl)aminodifluorphosphin, (Me3Si)2NPF2, erhält man unter Si—N-Bindungsspaltung Phosphazene vom Typ RF2P=N-PF2. Zu disubstituierten Tetracarbonylmolybdänkomplexen (RF2P=N—PF2)2Mo(CO)4 gelangt man durch Verdrängung des Cycloolefins aus C7H8Mo(CO)4 (C7H8 = Bicycloheptadien) mittels RF2P=N—PF2. (Me3Si)2NPF2 bildet ebenfalls einen Komplex [(Me3Si)2NPF2]2Mo(CO)4. Die genannten Verbindungen werden durch IR-, Massen-, 19F- und 31P-NMR-Spektren charakterisiert.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
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  • 8
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 504 (1983), S. 135-137 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Thermally Stable Trialkyl-2,2,2-trifluoro-1-(trifluoromethyl)-ethoxyphosphonium IodidesThe phosphinites R1R2POCH(CF3)2 (R1 = R2 = Me, tBu; R1 = Me, R2 = tBu) react with methyl iodide to give the thermally very stable phosphonium iodides [R1R2MePOCH(CF3)2]+I-. In the case of tBu2POCH(CF3)2 a sublimable 1:1 adduct is formed with boron trichloride.
    Notes: Die-Phosphinigsäureester R1R2POCH(CF3)2 (R1 = R2 = Me, tBu; R1 = Me, R2 = tBu) reagieren mit Methyliodid zu den thermisch sehr beständigen Phosphonium Iodiden [R1R2MePOCH(CF3)2]+I-. Im Falle von tBu2POCH(CF3)2 entsteht mit Bortrichlorid ein sublimierbares 1:1-Addukt.
    Additional Material: 1 Tab.
    Type of Medium: Electronic Resource
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  • 9
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 373 (1970), S. 182-188 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: By the reduction of C3F7Fe(CO)4J with sodium borohydride in methanol a solution is obtained from which derivatives of the very unstable perfluoropropyliron tetracarbonyl hydride C3F7Fe(CO)4H can be precipitated. The compounds [C3F7Fe(CO)4]2Hg and [C3F7Fe(CO)4]2[Fe(N2C12H8)3] have been characterized by their IR, NMR and mass spectra.
    Notes: Durch Reduktion einer Lösung von Heptafluor-n-propyl-eisen-tetracarbonyljodid, C3F7Fe(CO)4J, in Methanol mittels Natriumboranats entsteht eine Lösung, aus der Quecksilbercyanid und Tri-o-phenanthrolin-eisen(II)-sulfat Derivate des Heptafluor-n-propyl-eisentetracarbonylwasserstoffs, [C3F7Fe(CO)4]2Hg und [C3F7Fe(CO)(4)]2[Fe(N2C12H8)3] ausfällen. Aus dem Phenanthrolinderivat kann mittels Phosphorsäure das äußerst zersetzliche Carbonylhydrid C3F7Fe(CO)4H in Freiheit gesetzt werden. Die beiden beständigen Verbindungen sind durch IR-, NMR- und Massenspektren charakterisiert worden.
    Additional Material: 3 Tab.
    Type of Medium: Electronic Resource
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  • 10
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 522 (1985), S. 155-158 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On Sn[OCH(CF3)2]2 and Sn(OCH2CF3)2 (n = 1, 2)The sulfoxylates S[OCH(R)CF3]2, 1 and 2 and the disulfides S2[OCH(R)CF3]2, 5 and 6 (R = CF3, H) are obtained by reacting SCl2 or S2Cl2, respectively, and the lithium alcoxides LiOCH(R)CF3. Chlorine and compound 2 give ClS(O)OCH2F3 and CF3CH2Cl, whereas the sulfur-sulfur bound is cleaved in 5 and 6 furnishing SCI2, 1 and 2, respectively. The 19F n.m.r. spectrum of 5 and the 1H n.m.r. spectrum of 6 are interpreted in terms of hindered rotation about the sulfur-sulfur axis.
    Notes: Sulfoxylsäureester S[OCH(R)CF3]2, 1 und 2, sowie Disulfide S2[OCH(R)CF3]2, 5, und 6, (R = CF3, H) werden durch Umsetzung von Schwefeldichlorid bzw. Dischwefeldichlorid mit Lithiumalkoxiden LiOCH(R)CF3 erhalten. 2 setzt sich mit Chlor zu ClS(O)OCH2CF3 und CF3CH2Cl um, 5 und 6 ergeben unter Spaltung der Schwefel-Schwefel-Bindung SCl2 und 1 bzw. 2. Das 19F-NMR-Spektrum von 5 und das 1H-NMR-Spektrum von 6 geben Hinweise für eine gehinderte Rotation um die Schwefel-Schwefel-Bindung.
    Type of Medium: Electronic Resource
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