in tetrachloromethane pptn. of NH4Cl from a soln. of 3 g PCl5 in 1000 ml CCl4 half-saturated with gaseous NH3 at -3 °C; soln. contains (PNCl2)3 and (PNCl2)4;; evapn. of the mother liquor, fractional crystn. from toluene;;
in not given react. of 400 g PCl5 with 120 g NH4Cl in an inert solvent;; sucking off the formed mass, washing with ice-cold C6H6; fractional distn.; yield 50 percent (NPCl2)3, 25 percent (NPCl2)4 and 25 percent higher polymers;;
in dichloromethane byproducts: high oligomers; inert atmosphere; dropwise addn. of 1 equiv. PCl5 to amine at reflux, refluxing for 8 h; distn.; product mixt. not sepd., detd. by (31)P-NMR spectroscopy;
参考文献
Allcock, Harry R.; Crane, Chester A.; Morrissey, Christopher T.; Olshavsky, Michael A.
Inorganic Chemistry, 1999 , vol. 38, # 2 p. 280 - 283
in nitrobenzene small amount of azide; detected by NMR;
参考文献
Dillon, Keith B.; Platt, Andrew W. G.; Waddington, Thomas C.
Journal of the Chemical Society, Dalton Transactions: Inorganic Chemistry (1972-1999), 1981 , p. 2292 - 2295
in nitrobenzene small amount of azide; detected by NMR;
参考文献
Dillon, Keith B.; Platt, Andrew W. G.; Waddington, Thomas C.
Journal of the Chemical Society, Dalton Transactions: Inorganic Chemistry (1972-1999), 1981 , p. 2292 - 2295
Chistyakov, E. M.; Filatov, S. N.; Kireev, V. V.; Lysenko, K. A.; Buzin, M. I.; Chuev, V. P.
Russian Journal of General Chemistry, 2012 , vol. 82, # 6 p. 1065 - 1068,4
Zhurnal Obshchei Khimii, 2012 , vol. 82, # 6 p. 1065 - 1068,4
