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Darstellung und Eigenschaften von und Reaktionen mit metallhaltigen Heterocyclen, XIII. Darstellung und Kristallstrukturen neuartiger Mangana- und Rhenaphosphacycloalkane durch Substitution und reduktive Cycloeliminierung mit ω-Chlor-1-(diphenylphosphino)alkanen
Lindner, Ekkehard,Funk, Guido,Hoehne, Sigrud
, p. 2465 - 2478 (2007/10/02)
The three to six-membered mangana- and rhenaphosphacycloalkanes of the type are obtained by reductive cycloelimination of the phosphane complexes (OC)4BrMPPh2-n-Cl (3a - d, 3b' - d') with sodium amalgam . 3a - d are accessible in substituting CO by the phosphanes PPh2-n-Cl (2a - d) in BrMn(CO)5 (1), 3b' - d' by reaction of 2 (1') with 2b - d .The hitherto unknown phosphane PPh2-4-Cl (2d) is formed by action of NaPPh2 on Cl-4-Cl in THF and can easily be t ransformed with O2 into the oxide Cl-4-P(O)Ph2 (4d) .For the synthesis of 5c and 5c' the reaction of PPh2-3-MgCl with 1 and 1', respectively, is also suitable . 5b is thermally labile and reacts with PPh3 under CO insertion into the Mn - C ? bond to give the cyclic acyl derivative (6) . 5b' and 5c crystallize in the monoclinic space group P21/n and C2/c with Z = 4 and 8, respectively.
