in neat (no solvent)
29percent excess PF3 condensed onto Ni(allyl)2 and reagents allowed to react at 25°C for 1.5 h; react. mixt. fractionated, Ni(PF3)4 recovered in -80°C trap;
参考文献
Severson, Sarah J.; Cymbaluk, Teddy H.; Ernst, Richard D.; Higashi, John M.; Parry, Robert W.
Inorganic Chemistry, 1983 , vol. 22, p. 3833 - 3834
PF3 in 2-methyl cyclohexane
absence of air and moisture; condensing Ni-vapour into methylcyclohexanecontg. excess of PF3 and cycloheptatriene (-130°C); IR and mass spectroscopy;
参考文献
Timms, Peter L.; Turney, Terence W.
Journal of the Chemical Society, Dalton Transactions: Inorganic Chemistry (1972-1999), 1976 , p. 2021 - 2025
in neat (no solvent)
High Pressure; treating Ni-powder (prepd. by thermal decompn. of Ni-oxalate in N2- or H2-stream) in rotary autoclave (Cu-impeller) with PF3 (350 atm) for 42 h at 100 °C;; distilling off PF3 at -100 °C, further react. with PF3 for 16 h at 100 °C and 180 atm;;
参考文献
Kruck, T.; Baur, K.
Chemische Berichte, 1965 , vol. 98, p. 3070 - 3080
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;;
参考文献
Seel, F.; Ballreich, K.; Schmutzler, R.
Chemische Berichte, 1961 , vol. 94, p. 1173 - 1184
Full Text Show Details
Schmutzler, R.
Advan. Chem. Ser. Nr. 37 (1963) 150/60