in further solvent(s) dissolving PCl3 distd. under N2 in benzyl chloride distd. under N2; addn. of NH4Cl dryed in vac. and passing in the corresponding amount of Cl2; heating in a stream of N2 at 130 °C; removal of formed HCl by a stream of N2;; filtration, distg. off the solvent at 40 °C and 0.5 Torr; recrystn. from petroleum ether; product contains small amounts of higher polymers;;
in dichloromethane byproducts: PCl4(N3)(pyridine); 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 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
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 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
in tetrahydrofuran 9 h; Heating; Yield given. Further byproducts given. Yields of byproduct given. Title compound not separated from byproducts;
参考文献
Mitropol'skaya, G. I.; Kireev, V. V.; Korshak, V. V.; Goryaev, A. A.
J. Gen. Chem. USSR (Engl. Transl.), 1982 , vol. 52, # 11 p. 2486 - 2491,2197 - 2201
in neat (no solvent)
condensation of liquid SO2 on a mixt. of (NPCl2)4 and KF; heating at 98-100 °C for 22 days;; removal of an excess of SO2; fractionation;;
参考文献
Chapman, A. C.; Paddock, N. L.; Paine, D. H.; Searle, H. T.; Smith, D. R.
Journal of the Chemical Society, 1960 , p. 3608 - 3614
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Gmelin Handbook: P: MVol.C, 238, page 544 - 546
