in further solvent(s) addn. of 350 g Br2 to a mixt. of 300 g PBr2 and 250 g NH4Br in 450 ml (CHCl2)2 at 110-120 °C; heating at 145-155 °C for 2-3 days; colling; removal of remained NH4Br;; removal of the solvent at 35-40 °C and 2 Torr; removal of the oily compound of the crude product; sublimation at 130-160 °C and 0.05-0.5 Torr forming a mixt. of with more (NPBr2)3 than (NPBr2)4; fractional distn., chromatography (Al2O3);;
aluminium in solid liquid Br2 was dropped into a solid mixt. of oxide and a large excess ofAl powder in one-end sealed quartz tube under Ar atm., evacuated, seale d, placed in a tabular furnace with temp. gradient from 750 to 460 K;
参考文献
Wang, Zhi-Chang; Yu, Jin
Inorganic Chemistry, 2007 , vol. 46, # 10 p. 4248 - 4255
in carbon disulfide slowly mixing solns. of excess PBr3 and Br2 in CS2 with continuous stirring (to avoid formation of PBr7);; after decanting, crystals are washed with CHCl3 on a filter of fritted glass and stored in absence of air;;
Harries, G. S.; Payne, D. S.
Journal of the Chemical Society, 1956 , p. 4617 - 4621
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Gmelin Handbook: P: MVol.C, 218, page 501 - 503
