反应条件
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
Inorganic Syntheses, , vol. 6, p. 108 - 111
Brauer, G., Handbuch der praeparativen anorganischen Chemie, Stuttgart 1960, S. 522