sodium acetate in ethanol dissolving Ni-acetate in ethanol; addn. of stoich. amt. of acetylacetone in a soln. of sodium acetate; keeping the system in a boiling-water bath;; pptn., filtering, washing and drying;;
in solid solid-state synthesis from NiCl2 (14.7 mmol) and NaCH3COCHCOCH3 (27.0 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
→
反应条件
in diethyl ether byproducts: (PhSi(OH)O)6; acetylacetone was added to Ni compd. in Et2O; stirred at room temp. for 50 min; filtered; washed (Et2O); filtrate concd.; C6H6 added; filtered; dried inair; mother liquor evapd.; dried (vac.); elem. anal.;
参考文献
Sergienko; Cherkun; Myakushev; Korlyukov; Zavin
Russian Chemical Bulletin, 2010 , vol. 59, # 7 p. 1369 - 1375
