in neat (no solvent) heating mixture of 1 Mol I2 and 0.75 Mol red P and stirring for 1 h at 180°C after reaction took place;; dissolving in boiling chlorobenzene, filtering off, washing crystals with hot CHCl3 and drying in vacuum;;
in dichloromethane-d2 I2 was sublimed into the complex at 77 K after CH2Cl2, stored at -80°C and every 30 min heavily shaken for about 1 min (10 times), 4 days(inert atm.); ppt. was filtered at -80°C, volatiles were quickly removed at 0°C; elem. anal.;
参考文献
Krossing, Ingo
Journal of the Chemical Society, Dalton Transactions, 2002 , # 4 p. 500 - 512
trimethylsilyl iodide in carbon disulfide under N2, reaction of P4 with I2, followed by treatment of the soln. with (CH3)3SiI; not isolated, identified by 31P-NMR spectroscopy;
参考文献
Tattershall, Bruce W.; Kendall, Nigel L.
Polyhedron, 1994 , vol. 13, p. 1517 - 1522
