in neat (no solvent) reaction by redn. of V2O3 powder with an excess of Ca borings (50-150percent) in presence of CaCl2 as fluxing medium in an Ar atmosphere at temperatures above 1400 °C (ignition with high frequency heating);; metallic V with impurities;;
参考文献
Gregory, E. D.; Lilliendahl, W. C.; Wroughton, D. M.
Journal of the Electrochemical Society, 1951 , vol. 98, p. 395 - 399
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Gmelin Handbook: V: MVol.A1, 68, page 293 - 295
in neat (no solvent) reaction by heating of the mixture (with addition of Na or K) in a bomb at 900-950 °C for a period of 1 hour;; purification of the metal by isolation from the slags, formation of ductile V balls with a diameter up to 9 mm and a purity of 99.29-99.8percent;;
in tetrahydrofuran; diethyl ether; ammonia byproducts: CaCl2; NH3 (liquid); (N2); charging of Ca in dry box Schlenk tubes with (SnPh3)2; addn. of THF, cooling to -78°C; condensation of pre-dried liq. NH3 onto react. mixt., reflux for 6 h at -33°C; warming to room temp.; evapn. of NH3, addn. of 1N HCl soln. in Et2O; removal of volatiles in vac., dissolving in Et2O, filtration through Celite padded filter frit, removal of solvent;
参考文献
Journal of Organometallic Chemistry, , vol. 613, # 2 p. 139 - 147
