hydrogen bromide in pentane
Under stirring a strong stream of hydrogenhalogenide is bubbled for 10 min through the cooled (0°C) soln. of phosphine complex (inert atmosphere).; Solvent is evapd. at room temp. in vac., residue is digested with pentane, dialkylamminhydrohalogenide is filtered off, filtrate is dried to dryness in vac., recrystn. from pentane (-78°C), elem. anal.;
参考文献
Diemert, K.; Kuchen, W.; Lorenzen, D.
Journal of Organometallic Chemistry, 1989 , vol. 378, p. 17 - 32
hydrogen bromide in benzene
Under stirring a strong stream of hydrogenhalogenide is bubbled for 10 min through the cooled (0°C) soln. of phosphine complex (inert atmosphere).; Solvent is evapd. at room temp. in vac., residue is digested with pentane, dialkylamminhydrohalogenide is filtered off, filtrate is dried to dryness in vac., recrystn. from pentane (-78°C), elem. anal.;
参考文献
Diemert, K.; Kuchen, W.; Lorenzen, D.
Journal of Organometallic Chemistry, 1989 , vol. 378, p. 17 - 32
hydrogen bromide in benzene
Under stirring a strong stream of hydrogenhalogenide is bubbled for 10 min through the cooled (0°C) soln. of phosphine complex (inert atmosphere).; Solvent is evapd. at room temp. in vac., residue is digested with pentane, dialkylamminhydrohalogenide is filtered off, filtrate is dried to dryness in vac., recrystn. from pentane (-78°C), elem. anal.;
参考文献
Diemert, K.; Kuchen, W.; Lorenzen, D.
Journal of Organometallic Chemistry, 1989 , vol. 378, p. 17 - 32
in pentane
Under stirring a strong stream of HBr is bubbled at 0°C for 10 min to the cooled soln. of (Me2N)P(c-Hex)(Cr(CO)5).; Solvent is evapd. at room temp. in vac., residue is digested with pentane, filtered, filtrate is dried to dryness in vac., residue is taken off in pentane, chromy. (silica gel, pentane), elem. anal.;
参考文献
Diemert, K.; Kuchen, W.; Lorenzen, D.
Journal of Organometallic Chemistry, 1989 , vol. 378, p. 17 - 32
→
反应条件
in dichloromethane
under N2 mixt. Mo(HB(Me2pyz)3)(NO)Br2 and dimethylamine in dichloromethane stirred for 10 min; volume solvent reduced in vacuo, Et2O added, (NH2Me2)Br filtered off, filtrate evapd. in vacuo and allowed to stand at -5°C; elem. anal.;
参考文献
Drane, A. Stephen; McCleverty, Jon A.
Polyhedron, 1983 , vol. 2, p. 53 - 58
Appleton, David C.; Bull, David C.; Givens, Richard S.; Lillis, Veronica; Kenna, James Mc; et al.
Journal of the Chemical Society, Perkin Transactions 2: Physical Organic Chemistry (1972-1999), 1980 , p. 77 - 82