[PCl2(NP(C6H5)3)2]Cl in dichloromethane (N2); a soln. of Si compd. added dropwise to a soln. of PCl2(NP(C6H5)3)2Cl, stirred for 24 h at 25°C; not isolated, detected by NMR;
参考文献
Blackstone, Vivienne; Lough, Alan J.; Murray, Martin; Manners, Ian
Journal of the American Chemical Society, 2009 , vol. 131, p. 3658 - 3667
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 75 g (NPCl2)3, 25 g (NPCl2)4;;
in further solvent(s) dissolving PCl3 distd. under N2 in (CHCl2)2 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; products (NPCl2)3, (NPCl2)4 and a small amount of oily polymers;;
参考文献
Yokoyama, M.
Nippon Kagaku Kaishi (1921 - 47), 1959 , vol. 80, p. 1189 - 1191
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
