in acetylacetone byproducts: 1,3,5-trimethylbenzene, H2; under purified Ar atm.; V(η6-Me3C6H3)2 was dissolved in neat acetyl acetone; mixt. refluxeed for 5 hs; excess of acetyl acetone removed (vac., room temp.); residue suspended in heptane; suspn. filtered; dried (vac.) at room temp.;
参考文献
Calderazzo, Fausto; Englert, Ulli; Pampaloni, Guido; Volpe, Manuel
Journal of Organometallic Chemistry, 2005 , vol. 690, # 14 p. 3321 - 3332
in neat (no solvent) byproducts: H2; Electrolysis; exclusion of air; addn. of acetylacetone and (n-Bu4N)Br to electrolysisautoclave with V anode, current 100 mV, initial voltage of 8 V, electrolysis for 27 h; concn. (high vac.), recrystn., sublimation;
sodium carbonate in chloroform addition of 1.5 mol Na2CO3 in H2O to a solution of 3 mol acetyl acetone and 1 mol VCl3 in CHCl3 and evaporation;; crystallization; washing with cold alcohol and drying under CO2 on a water bath;;
参考文献
Journal of the Chemical Society, , vol. 103, p. 78 - 90
in solid solid-state synthesis from VCl3 (9.5 mmol) and NaCH3COCHCOCH3 (28.7 mmol) by mechanical activation (vibrating quartz vessel for 2 h at 5 Hz); transferring product into dry box under inert atmosphere;; vac. sublimation (0.1 torr) at 150-200°C bath temp.;;
参考文献
Borisov, A. P.; Petrova, L. A.; Makhaev, V. D.
Journal of General Chemistry USSR (English Translation), 1992 , vol. 62, p. 10 - 12
Zhurnal Obshchei Khimii, 1992 , vol. 62, p. 15 - 17
