144094-33-7Relevant articles and documents
Complexes of tert-butyl diphenylphosphinomethyl ketone N-phenylhydrazone, Z-PPH2CH2C(But)=NNHPH, with molybdenum, palladium or platinum: Crystal structure of cis-[PdCl2{Z-PPH2CH2C(Bu t)=NNHPH}2]
Ahmad, Mustaffa,Perera, Sarath D.,Shaw, Bernard L.,Thornton-Pett, Mark
, p. 59 - 67 (2008/10/08)
tert-Butyl diphenylphosphinomethyl ketone N-phenylhydrazone, Z-PPh2CH2C(But)=NNHPh (1), was prepared by heating the phosphino N,N-dimethylhydrazone, Z-PPh2CH2C(But)=NNMe2 with PhNHNH2 in ethanol in the presence of acetic acid as catalyst. This phosphine was converted into the corresponding phosphine oxide 2a and phosphine sulfide 2b. Treatment of [Mo(CO)4(nbd)] (nbd=norbornadiene) with 1 equiv. of 1 gave the tetracarbonylmolybdenum(0) complex [Mo(CO)4{PPh2CH2C(But)=NNHPh}] (3) in which 1 is bidentate; [Mo(CO)4(nbd)] with 2 equiv. of 1 gave the bis(phosphine)molybdenum(0) complex cis-[Mo(CO)4{PPh2CH2C(Bu t)=NNHPh}2] (4) in which 1 is monodentate through P. Treatment of [PdCl2(NCPh)2] or [PtCl2(cod)] (cod=cycloocta-1,5-diene) with 2 equiv. of 1 gave the complexes cis-[MCl2{PPh2CH2C(But)=NNHPh} 2] (M=Pd (5a), Pt (5b)). The crystal structure of 5a was determined. Treatment of [PtCl2(NCMe)2] with 2 equiv. of the phosphine 1 gave trans-[PtCl2{PPh2CH2C(Bu t)=NNHPh}2] (5c). Dehydrochlorination of the platinum(II) dichloride 5b or 5c with Et3N gave the neutral cis-[Pt{PPh2CH2C(But)=NNPh}2] (6), containing two six-membered chelate rings. Treatment of the π-2-methylallyl complex [{(η3-2-MeC3H4)PdCl}2] with 2 equiv. of the phosphine 1 gave the neutral complex [(η3-2-MeC3H4)PdCl{PPh2CH 2C(But)=NNHPh}] (7) in which 1 is monodentate through P. Dehydrochlorination of 7 with aqueous NaOH solution gave the π-methylallylpalladium(II) chelate complex [(η3-2-MeC3H4)Pd{PPh2CH 2C(But)=NNPh}] (8) containing an amidepalladium bond. Treatment of 1 with LiBun followed by PPh2Cl gave the diphosphine Z-PPh2CH2C(But)=NN(Ph)PPh2 (9) which with 0.5 equiv. of [{(η3-2-MeC3H4)PdCl}2] followed by NH4PF6 gave the π-methylallylpalladium(II) PF6 salt [(η3-2-MeC3H4) Pd-{PPh2CH2C(But)=NN(Ph)PPh 2}]PF6 (10). Crystals of 5a are monoclinic, space group P21/c, with a=12.900(2), b=40.083(6), c=10.8779(11) A, β=111.891(7)o and Z=4, final R=0.0535 for 7558 observed reflections with F>4.0σ(F).