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
→
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;;
in not given react. of PCl5 with OP(NH2)3 without removal of formed HCl; primary formation of OP(NH2)2Cl, condensation forming ((NH)2(POCl2)2)(n); further react. with PCl5 forming POCl3, NH3 and (PNCl2)(n);;
参考文献
Becke-Goehring, M.; Mann, T.; Euler, H. D.
Chemische Berichte, 1961 , vol. 94, p. 193 - 198
Full Text Show Details
Gmelin Handbook: P: MVol.C, 192, page 441 - 443
in not given
react. with OP(NH2)3; removal of formed HCl with dry air;;
参考文献
Becke-Goehring, M.; Mann, T.; Euler, H. D.
Chemische Berichte, 1961 , vol. 94, p. 193 - 198
Full Text Show Details
Gmelin Handbook: P: MVol.C, 192, page 441 - 443
