P6tBu4O and P7tBu5O— the First Polycyclophosphane Oxides

Baudler, M.; Michels, Martin; Pieroth, Manfred; Hahn, Josef

doi:10.1002/anie.198604711

Cited by 14 publications

(5 citation statements)

References 10 publications

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“…It has been found that the bicyclophosphanes PeBu( 72b) and P7But5 (93) in solution react with less than a stoichiometric amount of dry air at room temperature to form the monoxides 102/103 or 104/105, respectively. 344 When the stoichiometric amount of atmospheric oxygen is employed, the corresponding dioxides and other subsequent products are also formed. Both monoxides are produced as mixtures of two constitutional isomers (ratios 102/103 = 4.5:1; 104/105 ** 1:1);…”

Section: Polycyclophosphane Oxidesmentioning

confidence: 99%

Contributions to the chemistry of phosphorus. 218. Monocyclic and polycyclic phosphines

Baudler¹,

Glinka²

1993

Chem. Rev.

315

282

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Section: Polycyclophosphane Oxidesmentioning

confidence: 99%

Contributions to the chemistry of phosphorus. 218. Monocyclic and polycyclic phosphines

Baudler¹,

Glinka²

1993

Chem. Rev.

315

282

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“…Baudler and co‐workers reported on ( t Bu) 4 P 6 ( 1 , Scheme ) and the related oxide ( t Bu) 4 P 6 O ( 2 ), which were derived from t BuPCl 2 and PCl 3 by reduction with Mg and subsequent oxidation by exposure to air 14. 15 As reported by the group of Jutzi, thermolysis of (Cp*P) 3 yielded the structurally related bicyclic hexaphosphane Cp* 4 P 6 ( 3 , Cp*=pentamethylcyclopentadienyl) as well as the tricyclic hexaphosphane Cp* 2 P 6 ( 4 ), which incorporates a benzvalene type P 6 scaffold ( A ) 16. 17 Weigand and co‐workers reported on the cationic compound [Ph 4 P 6 ] 2+ ( 5 ), which can formally be derived from the prismane type structure ( B ) of P 6 18.…”

Section: Methodsmentioning

confidence: 99%

A Tricyclic Hexaphosphane

Bresien

Schulz

Villinger

2015

Chemistry A European J

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The reaction of the functionalized cyclo-tetraphosphane [ClP(μ-PMes*)]2 (Mes*=2,4,6-tri-tert-butylphenyl) with different Lewis bases led to the formation of an unprecedented tricyclic hexaphosphane, Mes*P6 Mes*. The formation of this compound was investigated by spectroscopic and theoretical methods, revealing an unusual ring expansion reaction. The title compound was fully characterized by experimental and computational methods.

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“…a,x-difunktionellen Organylpolyphosphans mit einem Di(halogen)organylphosphan bzw. Nach diesem Synthesekonzept konnte auch das monooxidierte Cyclotriphosphan (PBu t ) 3 O erhalten werden. Nach diesem Synthesekonzept konnte auch das monooxidierte Cyclotriphosphan (PBu t ) 3 O erhalten werden.…”

Section: O 1±4unclassified

“…Die Korrelation von MS-und 31 P-NMR-spektroskopischen Befunden ergibt das Vorliegen von zwei konstitutionsisomeren Dioxiden 2 a und 2 b, von denen 2 a auch als Zersetzungsprodukt von Tri-tert-butylcyclotriphosphan-monoxid, (PBu t ) 3 O, gebildet wird [1]. Detaillierte Aussagen zur Struktur von 2 a ergeben sich aus dem im 31 P{ 1 H}-NMR-Spektrum beobachteten AA'XX'-System (s. oben), dessen Signallagen auf einen P 4 -Ring mit zwei exocyclisch gebundenen Sauerstoffatomen hinweisen.…”

Section: (Pbu T ) 4 O (A B)unclassified

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Über die Oxo-cyclotetraphosphane (PBut)4O1-4

Baudler

Michels

2001

Z. anorg. allg. Chem.

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Professor Brigitte Sarry zum 80. Geburtstag gewidmet Inhaltsu È bersicht. Die Reaktion von Tetra-tert-butylcyclotetraphosphan, (PBu t ) 4 , mit trockenem Luftsauerstoff fu È hrt unter geeigneten Bedingungen zu dem entsprechenden Monoxid (PBu t ) 4 O (1), das sa È ulenchromatographisch isoliert werden konnte. Mit Wasserstoffperoxid wird ein Gemisch von Oxo-cyclotetraphosphanen (PBu t ) 4 O 1±4 gebildet, in dem neben 1 zwei konstitutionsisomere Dioxide (PBu t ) 4 O 2 (2 a, 2 b), das Trioxid (PBu t ) 4 O 3 (3) und das Tetroxid (PBu t ) 4 O 4 (4) vorliegen. Nach den 31 P-NMR-Parametern ist Sauerstoff ausschlieûlich exocyclisch an den Phosphor-Vierring gebun-den. Welche der P-Atome als k 5 -Phosphor vorliegen, geht aus der unterschiedlichen Tieffeldverschiebung der Signale fu È r die einzelnen P-Kerne gegenu È ber der Ausgangsverbindung hervor. Demnach ist 1 1,2,3,4-Tetra-tert-butyl-1-oxocyclotetraphosphan, 2 a und 2 b sind 1,2,3,4-Tetra-tertbutyl-1,2-dioxo-bzw. -1,3-dioxocyclotetraphosphan, 3 ist 1,2,3,4-Tetra-tert-butyl-1,2,3-trioxo-cyclotetraphosphan, und 4 ist 1,2,3,4-Tetra-tert-butyl-1,2,3,4-tetraoxo-cyclotetraphosphan. Bei fortschreitender Oxidation findet eine Spaltung des P 4 -Ringes statt. Contributions to the Chemistry of Phosphorus. 243 On the Oxocyclotetraphosphanes (PBu t ) 4 O 1±4Abstract. Under suitable conditions, the reaction of tetratert-butylcyclotetraphosphane, (PBu t ) 4 , with dry atmospheric oxygen gives rise to the corresponding monoxide (PBu t ) 4 O (1) which has been isolated by column chromatography. The reaction with hydrogen peroxide furnishes a mixture of oxocyclotetraphosphanes (PBu t ) 4 O 1±4 consisting of two constitutionally isomeric dioxides (PBu t ) 4 O 2 (2 a, 2 b), the trioxide (PBu t ) 4 O 3 (3), and the tetraoxide (PBu t ) 4 O 4 (4), in addition to 1. According to the 31 P NMR parameters the oxygen atoms are exclusively exocyclically bonded to the phosphorus four-membered ring. Which of the P atoms are present as k 5 -phosphorus follows from the different low-field shifts of the individual P nuclei compared with the starting compound. Accordingly, 1 is 1,2,3,4-Tetra-tert-butyl-1-oxocy-clotetraphosphane, 2 a and 2 b are 1,2,3,4-Tetra-tert-butyl-1,2dioxo-and -1,3-dioxocyclotetraphosphane, respectively, 3 is 1,2,3,4-Tetra-tert-butyl-1,2,3-trioxocyclotetraphosphane, and 4 is 1,2,3,4-Tetra-tert-butyl-1,2,3,4-tetraoxocyclotetraphosphane. When the oxidation reaction proceeds a fission of the P 4 ring takes place. Im Unterschied zu der betra È chtlichen Anzahl monocyclischer und polycyclischer Organylphosphane P n R m (m £ n) [2], die im allgemeinen durch Luftsauerstoff leicht oxidativ angegriffen werden, war u È ber die dabei gebildeten Sauerstoffderivate la È ngere Zeit nichts Na Èheres bekannt. Vor allem interessierte die Frage, ob Sauerstoff unter Insertion in das Phosphorgeru È st wie bei der Bildung von P 4 O 6 aus P 4 oder unter exocyclischer Addition an das intakte P n -Geru È st reagiert. Wir haben daher vor einiger Zeit eingehende Untersuchungen u È ber die Oxidationsprodukte...

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P₆tBu₄O and P₇tBu₅O— the First Polycyclophosphane Oxides

Cited by 14 publications

References 10 publications

Contributions to the chemistry of phosphorus. 218. Monocyclic and polycyclic phosphines

Contributions to the chemistry of phosphorus. 218. Monocyclic and polycyclic phosphines

A Tricyclic Hexaphosphane

Über die Oxo-cyclotetraphosphane (PBut)4O1-4

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