water in chloroform; ammonia addn. of a soln. of PCl5 in CHCl3 in liquid NH3 containing H2O; dissoilving the product in liquid NH3;; removal of formed NH4Cl with diethylamine and extraction with hot methanol;;
water in neat (no solvent) addn. of powdered PCl5 to liquid NH3 containing a small amount of H2O; primary react. of PCl5 with NH3 forming HNP(NH2)3;; OP(NH2)3, PH6ON3 and P3O2N8H13 are isolated;;
in chloroform satd. of 1500 ml freshly distd. CHCl3 with dry NH3 at -15 °C; addn. of a soln. of 60 g freshly distd. POCl3 in 100 ml CHCl3 drop by drop on cooling and stirring; passing in NH3 for 1 h; sucking off the ppt. after 12 h; washing with dry CHCl3;; drying in vacuum; removal of formed NH4Cl by react. with diethylamine forming insoluble (C2H5)2NH2Cl; recrystn. from methanol;;
参考文献
Gmelin Handbook: P: MVol.C, 156, page 356 - 358
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反应条件
in not given formation of a mixt. of PO(NH2)3, CaO and NH4Cl by react. of NH3 with CaO*2POCl3;;
