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 further solvent(s) react. of PCl5 with NH4Cl in (CHCl2)2;; recrystn. of the fraction containing (NPCl2)4 (180-187 °C at 10 Torr) from ethyl ether under discoloration of coal;;
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 further solvent(s) NH4Cl reacted with PCl5 in 1,1,2,2-tetrachloroethane according to L. G. Lund, N. L. Paddock, J. E. Proctor, H. T. Searle, Journal of the Chemical Society (1960) 2542; vac. distilled on Vigreux column;
参考文献
Vorontsov, Ivan I.; Tur, Dzidra R.; Papkov, Vladimir S.; Antipin, Mikhail Yu.
Journal of Molecular Structure, 2009 , vol. 928, # 1-3 p. 1 - 11
in trichlorophosphate byproducts: Cl2(O)P(NPCl2)5Cl; under reflux; treatment of the crude product with n-heptane, products identified in the sol. and in the insol. phase with NMR spectroscopy;
参考文献
Abouchaccra, Taher; Helioui, Moncef; Puskaric, Emile; Jaeger, Roger de; Heubel, Joseph
Journal of Chemical Research, Synopses, 1981 , p. 230 - 231
