phosphorus trichoride in neat (no solvent) passing dry Cl2 (dryed over H2SO4) in a suspension of red P (dryed over H2SO4) in PCl3; use of a glass apparatus with reflux condenser and P2O5 drying tube; boiling PCl3 during the rect. to prevent formation of PCl4;;
参考文献
Gmelin Handbook: P: MVol.C, 179, page 412 - 414
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Forbes, M. C.; Roswell, C. A.; Maxson, R. N.
Fernelius, W. C., Inorganic Syntheses, Bd. 2, New York-London 1946, S. 145/7
titanium; silicon in not given byproducts: POCl3, TiCl4; react. of ferrophosphorus containing Ti and Si with Cl2;;
参考文献
US2797980 , ;
C. A., , p. 15080
DE1065817 , ;
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DE1040516 , ;
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GB812801 , ;
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反应条件
acetonitrile in neat (no solvent) molar ratio tungsten ditelluride/PCl5 1/8; heated in evacuated sealed ampoules for 2 h at 170°C, cooled; PCl3 removed in a vac. at 80°C, extd. with hot acetonitrile, soln. cooled to -5°C; the residue dried in a vac.; NMR, mass, IR and Raman spectra;
参考文献
Russian Journal of Inorganic Chemistry (Translation of Zhurnal Neorganicheskoi Khimii), , vol. 32, p. 1049 - 1051
Zhurnal Neorganicheskoi Khimii, , vol. 32, p. 1769 - 1771
