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Synthese, Struktur und dynamisches Verhalten von 1,3,5-Triaza-2,4-diphospha-1,4-pentadienenVorgetragen auf der XIth International Conference on Phosphorus Chemistry, Tallinn, USSR, July 1989. (1990)

Niecke, Edgar ; Detsch, Ralph ; Nieger, Martin

Weinheim : Wiley-Blackwell

Berichte der deutschen chemischen Gesellschaft 123 (1990), S. 797-799

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ISSN: 0009-2940

Keywords: 1,3,5-Triaza-2,4-diphospha-1,4-Pentadienes, dynamic behavior ; Chemistry ; Inorganic Chemistry

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: Synthesis, Molecular Structure, and Dynamic Behaviour of 1,3,5-Triaza-2,4-diphospha-1,4-pentadienesChloro(arylimino)phosphane (1) reacts with the 1,3-diaza-2-phosphaallylic system 3 to form 1,3,5-triaza-2,4-diphospha-1,4-pentadienes Ar-N=P-N(R)-P=N-Ar (Ar = 2,4,6-tBu3-C6H2; R = tBu, 2,4,6-iPrc3C6H2) (4a-c). the molecular structure of 4a (“Exo-endo-S conformation”) as well as the dynamic behaviour of the compounds in solution are discussed. the observed temperature dependance of the NMR spectra of 4c was interpreted as a sigmatropic 1,3-rearrangement followed by a P-N rotation.

Additional Material: 1 Ill.

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1002/cber.19901230425

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Synthese und Reaktivität eines 1-Chlor-λ3-phosphirans (1989)

Niecke, Edgar ; Leuer, Martina ; Nieger, Martin

Weinheim : Wiley-Blackwell

Berichte der deutschen chemischen Gesellschaft 122 (1989), S. 453-461

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ISSN: 0009-2940

Keywords: 1-Chloro-2,2,3-tris(trimethylsilyl)phosphirane ; Phosphirane derivatives ; Chemistry ; Inorganic Chemistry

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Description / Table of Contents: Synthesis and Reactivity of a 1-Chloro-λ3-phosphirane[Bis(trimethylsilyl)methyl]dichlorophosphane (1) reacts with chlorobis(trimethylsilyl)methyllithium (2) to give 1-chloro-λ3-phosphirane 6. Nucleophilic substitution of the chlorine atom of 6 leads to a variety of derivatives 9a-n. In the case of bis(trimethylsilyl)amine the reaction does not provide the aminophosphirane 15 but to the isomeric phosphaalkene 16. However, 15 is accessible by reaction of the methylenphosphane 17 with 2. With an excess of nucleophile 9 is cleaved to give the phosphide 13 and tris(trimethylsilyl)ethene (10). Phosphirane 9f dissociates thermically to give 10 and chloromethylenephosphane 20. Reaction of 6 with methylenetriphenylphosphorane and 1,8-diazabicyclo[5.4.0]undec-7-ene (DBU) leads to substitution with formation of 22, 23 while with trimethylsilyl azide the product is an azidophosphirane 24. 1-Chlorophosphirane 6 reacts with AlCl3 to give the phosphirane complex 27. The molecular structure of 27 as well as the NMR data of the phosphiranes are discussed.

Notes: [Bis(trimethylsilyl)methyl]dichlorphosphan (1) reagiert mit Chlorbis(trimethylsilyl)methyllithium (2) zu dem 1-Chlor-λ3-phosphiran 6. Durch nucleophile Substitution des Chloratoms läßt sich 6 vielfältig derivatisieren (9a-n). Im Falle der Umsetzung mit Bis(trimethylsilyl)amin führt die Reaktion nicht zum Aminophosphiran 15, sondern zum isomeren Phosphaalken 16. Phosphiran 15 ist jedoch durch Reaktion des Methylenphosphans 17 mit 2 zugänglich. Durch Nucleophil im Überschuß wird 9 unter Abspaltung von Tris(trimethylsilyl)ethen (10) zum Phosphid 13 gespalten. 9f zerfällt thermisch unter Bildung von 10 und Chlormethylenphosphan 20. 1,8-Diazabicyclo[5.4.0]undec-7-en (DBU) und Methylentriphenylphosphoran reagieren mit 6 unter Substitution zu 22 und 23, während mit Trimethylsilylazid ein Azidophosphiran 24 erhalten wird. AlCl3 reagiert mit 6 zum Phosphiran-Komplex 27. Die Molekülstruktur von 27 und die NMR-Daten der Phosphirane werden diskutiert.

Additional Material: 2 Ill.

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1002/cber.19891220310

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Bis(pentamethylcyclopentadienyl)-Substituted Phosphanes: Synthesis and Structure (1998)

Ebels, Jörg ; Pietschnig, Rudolf ; Kotila, Sirpa ; [et al.]

Weinheim : Wiley-Blackwell

Berichte der deutschen chemischen Gesellschaft 1998 (1998), S. 331-337

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ISSN: 1434-1948

Keywords: Bis(pentamethylcyclopentadienyl)phosphanes ; Aminobis(pentamethylcyclopentadienyl)phosphanes ; Chemistry ; General Chemistry

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: The bis(1,2,3,4,5-pentamethyl-1,3-cyclopentadien-1-yl)phosphanes 3-7 are formed in good yields by the reaction of the halogenophosphanes 2a or 2b with the appropriate nucleophile. Following another route, the dialkylaminobis(pentamethylcyclopentadienyl)phosphanes 11a-c have been synthesized by the treatment of dichloro(dialkylamino)phosphanes with two equivalents of (pentamethylcyclopentadienyl)lithium. The compounds 3-11 have been characterized by multinuclear NMR spectroscopy and 3, 5, 6, and 11a have also been characterized by single-crystal X-ray diffraction studies. The molecular structure of 11a is governed by steric congestion, which typically would lead to a parallel arrangement of the two pentamethylcyclopentadienyl ligands at the phosphorus atom. However, surprisingly, the crystal structure of the (dimethylamino)phosphane 11a, exhibits a tilted, rather than a parallel, conformation of the pentamethylcyclopentadienyl groups [tilt angle: 130.6(1)°].

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Synthesis and Crystal Structures of P-Halogeno(imino)methylenephosphoranes X-P(=NtBu3C6H2)=C(SiMe3)2 (X = Cl, Br, I) (1998)

Ruban, Alexander ; Nieger, Martin ; Niecke, Edgar

Weinheim : Wiley-Blackwell

Berichte der deutschen chemischen Gesellschaft 1998 (1998), S. 83-85

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ISSN: 1434-1948

Keywords: Phosphorus ylides ; Bis(ylene)phosphoranes ; Halogenophosphoranes ; X-ray structure analysis ; Chemistry ; General Chemistry

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: The iminophosphane (Me3Si)3C-P=N-Mes* (1) reacts with iodine to form the imino(methylene)phosphorane I-P(=N-Mes*)=C(SiMe3)2 (2). Upon subsequent treatment with AgCl, the corresponding chloro derivative 3 is obtained. Chlorine/bromine exchange in 3 with bromotrimethylsilane affords the bromo analogue 4. The structures of 2, 3 and 4 were confirmed by X-ray crystal structure analysis; each of the compounds features a trigonal-planar phosphorus atom.

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Ein Phosphor(III)-Derivat mit sterisch fixierter Bis(trimethylsilyl)amino-Gruppierung (1976)

Niecke, Edgar ; Flick, Wilhelm ; Pohl, Siegfried

Weinheim : Wiley-Blackwell

Zeitschrift für die chemische Industrie 88 (1976), S. 305-306

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ISSN: 0044-8249

Keywords: Chemistry ; General Chemistry

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Additional Material: 1 Ill.

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1002/ange.19760880916

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Phosphor(V) mit trigonal-planarer Koordination (1975)

Pohl, Siegfried ; Niecke, Edgar ; Krebs, Bernt

Weinheim : Wiley-Blackwell

Zeitschrift für die chemische Industrie 87 (1975), S. 284-285

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ISSN: 0044-8249

Keywords: Chemistry ; General Chemistry

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1002/ange.19750870805

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1,2-Cycloadditionsreaktionen an „Phosphazenen“ mit ungewöhnlicher Koordinationszahl: λ5-Phosphiran und 1,2λ5-AzaphosphiridinAuszugsweise vorgetragen beim 2nd Symp. Inorg. Phosphorus Compounds in Prag, September 1974. Diese Arbeit wurde von der Deutschen Forschungsgemeinschaft unterstützt. (1975)

Niecke, Edgar ; Flick, Wilhelm

Weinheim : Wiley-Blackwell

Zeitschrift für die chemische Industrie 87 (1975), S. 355-356

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ISSN: 0044-8249

Keywords: Chemistry ; General Chemistry

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1002/ange.19750870917

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1,3,2λ2,4-Diazaphosphoniaaluminatacyclobutan: Ein cyclisches Zwitterion mit zweifach koordiniertem PhosphorProfessor Oskar Glemser zum 65. Geburtstag gewidmet (1976)

Niecke, Edgar ; Kröher, Rainer

Weinheim : Wiley-Blackwell

Zeitschrift für die chemische Industrie 88 (1976), S. 758-759

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ISSN: 0044-8249

Keywords: Chemistry ; General Chemistry

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Additional Material: 1 Tab.

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1002/ange.19760882206

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Struktur des 1 : 1-Addukts aus Aminoiminophosphan und tert-Butylazid (1978)

Pohl, Siegfried ; Niecke, Edgar ; Schäfer, Hans-Günther

Weinheim : Wiley-Blackwell

Zeitschrift für die chemische Industrie 90 (1978), S. 135-136

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ISSN: 0044-8249

Keywords: Chemistry ; General Chemistry

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Additional Material: 1 Ill.

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1002/ange.19780900220

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Neuartige Diylide mit Phosphor der Koordinationszahl 315. Mitteilung über Untersuchungen an Phosphazenen der Koordinationszahl 2 und 3. Diese Arbeit wurde vom Fonds der Chemischen Industrie unterstützt. - 14. Mitteilung: E. Niecke, R. Kröher, S. Pohl, Angew. Chem. 89, 902 (1977); Angew. Chem. Int. Ed. Engl. 16, 864 (1977). (1978)

Niecke, Edgar ; Wildbredt, Dirk A.

Weinheim : Wiley-Blackwell

Zeitschrift für die chemische Industrie 90 (1978), S. 209-210

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ISSN: 0044-8249

Keywords: Chemistry ; General Chemistry

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Additional Material: 1 Tab.

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1002/ange.19780900311

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