13455-00-0Relevant articles and documents
Substitution of conventional high-temperature syntheses of inorganic compounds by near-room-temperature syntheses in ionic liquids
Groh, Matthias F.,Muller, Ulrike,Ahmed, Ejaz,Rothenberger, Alexander,Ruck, Michael
, p. 1108 - 1122 (2013)
The high-temperature syntheses of the low-valent halogenides P2I4, Te2Br, a-Te4I4, Te4(Al2Cl7)2, Te4(Bi6Cl20), Te8(Bi4Cl14), Bi8(AlCl4)2, Bi6Cl7, and Bi6Br7, as well as of WSCl4 andWOCl4 have been replaced by resource-efficient low-temperature syntheses in room temperature ionic liquids (RTILs). The simple one-pot syntheses generally do not require elaborate equipment such as twozone furnaces or evacuated silica ampoules. Compared to the published conventional approaches, reduction of reaction time (up to 80%) and temperature (up to 500 K) and, simultaneously, an increase in yield were achieved. In the majority of cases, the solid products were phase-pure. X-Ray diffraction on single crystals (redetermination of 11 crystal structures) has demonstrated that the quality of the crystals from RTILs is comparable to that of products obtained by chemical transport reactions.
Doughty, H. W.
, p. 1444 - 1445 (1905)
Preparation and spectroscopic characterization of difluorophosphorane, PH3F2. 31P NMR spectrum of protonated diphosphine, P2H5+
Minkwitz, Rolf,Liedtke, Andreas
, p. 4238 - 4242 (2008/10/08)
The preparation of difluorophosphorane, PH3F2, from the reaction of diphosphine and hydrogen fluoride is reinvestigated; it has been characterized by multinuclear (1H, 19F, 31P) NMR spectroscopy. Complete infrared and Raman low-temperature spectra of difluorophosphorane are reported. It reacts with alkali-metal fluorides to give phosphine and hexafluorophosphates(V). On the basis of 31P NMR spectroscopic results, a reaction mechanism for the formation of PH3F2 is proposed. The byproducts of the reaction were PH2F3, (PH)n, and P2H5+; the last was observed for the first time. In carbon disulfide solution, diphosphine neither reacts with hydrogen halides to yield protonated diphosphine nor interacts with hydrogen fluoride to form difluorophosphorane.
