carbon monoxide in diethyl ether High Pressure; under nitrogen; autoclave: 70 h at room temperature and 50 atm CO; then 1-2 h at 80-100 °C;; products were isolated by crystallization and chromatography; NMR, IR, MS;
参考文献
Journal of Organometallic Chemistry, , vol. 355, p. 243 - 256
carbon monoxide in diethyl ether High Pressure; under dried N2; addn. of N-methylbenzimine at 25°C to a soln. of W-complex (CO-pressure: 50 atm); stirring for 2 d at room temp., then for 1-2 h at 80-100°C; vac.-evapn. until dryness; residue dissolved in petroleum ether/ether; chromy. (silica gel/petroleum ether/ether); recrystn. from petroleum ether; elem. anal.;
参考文献
Journal of Organometallic Chemistry, , vol. 373, p. 203 - 220
water in THF-d8 (tetrahydrofuran-d8) Ar atmosphere; hydrolysis, room temp., 24 h; not isolated, ratio of (2,2,3-trimethylhept-5-en-3-on)/(2,3-3-trimethylhept-6-en-3-on) 45:55; (1)H-NMR spectroscopy;
in tetrahydrofuran byproducts: Me2S; under N2; W-complex in THF added to Fe-complex in THF, stirred overnight at room temp.; dried (vac.), dissolved in CH2Cl2, chromy. (alumina; eluent: CH2Cl2:petrolether = 1:1 (v/v)), crystn.;
THF in tetrahydrofuran Irradiation (UV/VIS); W2 complex in THF photolysed for 60 h with CF3C2CF3; chromd. (Florisil, hexane-CH2Cl2); elem. anal.;
参考文献
Guerchais, Jacques E.; LeQuere, Jean L.; Petillon, Francois Y.; Manojlovic-Muir, Ljubica; Muir, Kenneth W.; Sharp, David W. A.
Journal of the Chemical Society, Dalton Transactions: Inorganic Chemistry (1972-1999), 1982 , p. 283 - 290