14984-74-8Relevant academic research and scientific papers
1,3,2-Dithiaphospholanes with an annelated 1,2-dicarba-closo- dodecaborane(12) unit: Formation and reactivity
Wrackmeyer, Bernd,Klimkina, Elena V.,Milius, Wolfgang
, p. 5021 - 5043 (2014/04/03)
1,3,2-Dithiaphospholanes were prepared, containing an annelated 1,2-dicarba-closo-dodecaborane(12) unit, bearing halogens (F, Cl, Br, and I), H, NEt2, OEt groups, or organo substituents (R = i-Pr, t-Bu, Cy, 3,5-Me2-C6H3-CH2, Ph) at phosphorus. The t-Bu derivative was structurally characterised as its sulfide. The organo-substituted derivatives escape the ring strain by irreversible (R = t-Bu; X-ray analysis) or reversible dimerisation, by which 10-membered rings are formed. Using 1,1-bis(dichlorophosphino)methane, another dimer containing a 14-membered ring could be isolated and structurally characterised. The preferred conformation of the 1,3,2-dithiaphospholanes depends on the nature of the substituent at phosphorus. For instance, the substituents R = t-Bu, NEt 2 prefer the equatorial position, as indicated by diagnostic NMR data, supported by DFT calculations [B3LYP/6-311+G(d,p) level of theory]. The calculations also predict the tendency for dimerisation, and calculated NMR parameters are in good agreement, in most cases, with experimental data.
Preparation of new bis(dialkylamino)phosphine species via reduction of bis(dialkylamino)halophosphines
Snow, Sarah S.,Jiang, De-Xiang,Parry, Robert W.
, p. 1460 - 1463 (2008/10/08)
Four new bis(dialkylamino)phosphine species, (Me2N)2PH, CH3NCH2CH2N(CH3)PH, (CO)3Ni[(Me2N)2PH], and (CO)3Ni-[CH3NCH2CH2N(CH 3)PH], have easily been prepared in good yields through reduction of corresponding bis(dialkylamino)-halophosphines by lithium tri-sec-butylborohydride. The preparation and characterization of these compounds are discussed. An improved synthesis for obtaining quantitative yields of (CO)3NiL [L = Me2NPF2, (Me2N)2PF, CH3NCH2CH2N(CH3)PF] is also described.
