in hexane
Mo2(O-i-Pr)6 was dissolved in hexane. This soln. was cooled to -21°C, and then a hexane soln. of iodotrimethylsilane was added to the stirring soln.. The soln. was stirred at -21°C for 2 h.; The soln. was then allowed to warm to room temp. and stirred another 4 h, to yield a microcrystalline ppt.. The mixt. was then cooled to -15°C, and small crystals were isolated after 1 d.;
参考文献
Chisholm, Malcolm H.; Clark, David L.; Errington, R. John; Folting, Kirsten; Huffman, John C.
Inorganic Chemistry, 1988 , vol. 27, p. 2071 - 2084
in toluene
Under N2, Mo2(O-i-Pr) was dissolved in toluene, and the mixt. was cooled to -78°C. Iodotrimethylsilane was added, and the react. mixt. was stirred and warmed to 0°C. After 2 h the soln. was allowed to warm to room temperature.; The soln. was reduced in vol. by half and cooled to -15°C for 24 h, which yielded crystals. After 2 d, crystals were isolated by filtration and dried in vacuo. Traces of Mo4O2I2(O-i-Pr)6 present in Mo4I4(O-i-Pr)8; detd. by (1)H-NMR.;
参考文献
Chisholm, Malcolm H.; Clark, David L.; Errington, R. John; Folting, Kirsten; Huffman, John C.
Inorganic Chemistry, 1988 , vol. 27, p. 2071 - 2084
in toluene
Mo2(O-i-Pr)6 was dissolved in toluene uner N2, and the mixt. was cooled to -78°C. Iodotrimethylsilane was added dropwise. The soln. was allowed to warm to room temp.. After 3 h at room temp. the mixt. was warmed to 55°C and stirred (2 d).; The soln. was reduced in vol. by half and cooled to -15°C. After 2 d a ppt. was isolated by filtration and dried in vacuo.;
参考文献
Chisholm, Malcolm H.; Clark, David L.; Errington, R. John; Folting, Kirsten; Huffman, John C.
Inorganic Chemistry, 1988 , vol. 27, p. 2071 - 2084
Blackburn, G. Michael; Ingleson, David
Journal of the Chemical Society, Perkin Transactions 1: Organic and Bio-Organic Chemistry (1972-1999), 1980 , p. 1150 - 1153
2 h at -5 deg C, then 5 h at 30 deg C; Product distributionMechanism;
参考文献
Voronkov, M. G.; Dubinskaya, E. I.; Sigalov, M. V.; Vitkovskii, V. Yu.
J. Gen. Chem. USSR (Engl. Transl.), 1989 , vol. 59, # 5.1 p. 1055 - 1057,932 - 933
