SbF5 in neat (no solvent)
react. of (Ni(PCl3)4) with SBF3 in presence of catalytic amt. of SbF5;;
参考文献
Wilkinson, G.
Am. Chem. Soc., 1951 , vol. 73, p. 5501 - 5502
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Gmelin Handbook: Ni: MVol.C1, 3, page 11 - 13
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Wilkinson, G.
N. S. A., NP-1857 (1951) 1/173 1951 , vol. 5, p. 4093
in further solvent(s)
byproducts: SO2; react. of KSO2F with (Ni(PCl3)4) under exclusion of air and moisture in m-dichlorobenzene (cooling with ice), stirring for 30 min at ambient temp. and for 2 h at 90 °C;; collecting volatile react. products in cooled U-tube (filled with KSO2F), distilling into second U-tube after evapn. of SO2, distillation of (Ni(PF3)4) in micro-column at 760 torr under N2;;
in neat (no solvent)
byproducts: PCl3; heating (Ni(PCl3)4) with excess of PF3 in closed tube for 24 h on steam bath, cooling react. tube with liq. N2 after the react. is finished and distilling off PF3 at -115 °C (vac.), raising temp. to 0 °C;; sepg. upper layer of PCl3 from (Ni(PF3)4), fractional distillation in high vac. with addn. of SbF3 and traces of SbF5;;
参考文献
Wilkinson, G.
Am. Chem. Soc., 1951 , vol. 73, p. 5501 - 5502
Full Text View citing articles Show Details
Gmelin Handbook: Ni: MVol.C1, 3, page 11 - 13
Full Text Show Details
Wilkinson, G.
N. S. A., NP-1857 (1951) 1/173 1951 , vol. 5, p. 4093