in diethyl ether reduction of PCl3 with LiAlH4 in ether at 0 °C;;
参考文献
Paddock, N. L.
Nature (London, United Kingdom), 1951 , vol. 167, p. 1070 - 1071
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Saalfeld, F. E.; Svec, H. J.
C. A., IS-386 (1961) 68/77 1962 , p. 236
sodium hydride in mineral oil reduction of PCl3 with NaH and B(C2H5)3 in mineral oil at -10-30 °C; formation of Na(BH(C2H5)3) as intermediate and reducing agent;; sukking off PH3 in vacuum;;
water; sodium hydrogencarbonate in water byproducts: Na3HP2O6; hydrolysis; passing a stream of N2 containing gaseous PCl3 in a suspension of NaHCO3 in H2O on cooling with ice; primary formation of phosphite Na2HPO3; react. of Na2HPO3 forming pyrophosphite Na3HP2O5;; formation of diphosphate Na2H2P2O7, hypophosphate Na3HP2O6, monophosphate Na2HPO4, a small amount of iso-hypophosphate Na3HP2O6 and PH3; mechanism described;;
参考文献
Thilo, E.; Heinz, D.
Z. anorg. allg. Chem., 1955 , vol. 281, p. 303 - 321
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Gmelin Handbook: P: MVol.C, 183, page 421 - 424
in tetrahydrofuran byproducts: LiCl, H2; Ar atmosphere, addn. of soln. of PCl3 (-78°C) to suspn. of LiH (-40°C, over 45 min, stirring); filtn., removal of PH3 (-60°C, vacuum), filtn.; not isolated, soln. contg. ca. 10percent impurities;
in ethylene glycol dimethyl ether byproducts: (SiH2)(n); under N2, soln. of KSiH3 is introduced via a syringe and septum into a vessel in which PCl3 is condensed at -196°C, mixt. is warmed to room temp.;
参考文献
Williams, Victor A.; Ritter, David M.
Inorganic Chemistry, 1985 , vol. 24, p. 3278 - 3280