199620-14-9合成路线 (共 107 条)
反应条件
in decalin byproducts: CO; 3.5:1 mixture of arene and Cr(CO)6 in solvent purged for 20 min with Ar, evacuated for 20 min, mixture refluxed, cooled to 20°C, cooled to -18°C under argon, reaction time 5 h; filtered off, dissolved in benzene, filtered through Kieselguhr, concentrated, light petroleum added, crystn. at -18°C, complexes eluted with benzene/ethyl acetate, elem. anal., NMR;
参考文献
Journal of Organometallic Chemistry, , vol. 393, # 1 p. 115 - 118
反应条件
in Petroleum ether boiling;;
参考文献
Gmelin Handbook: Cr: Org.Verb., 1.6.1.3.1.1, page 290 - 297
反应条件
in anhydrous butyl ether N2-atmosphere; refluxing for 40 h (returning of Cr(CO)6 from condenser to flask by mechanical scrapping); filtration (Celite), evapn. (reduced pressure), thin layer chromy. (SiO2, CH2Cl2/light petroleum=1:9);
参考文献
Journal of the Chemical Society, Dalton Transactions: Inorganic Chemistry (1972-1999), , p. 1874 - 1880
反应条件
in tetrahydrofuran; anhydrous butyl ether The ester and Cr(CO)6 were treated with dibutyl ether and then THF, and the soln. was refluxed (N2). The react. was monitored by thin layer chromy. (C6H12/ether, 9/1).; Filtration, evapn. of solvent; Flash chromy. and development with hexane resolved 2 bands; 1. band, C6H6Cr(CO)3, 2. band mixt. of diastereomers (90percent, α/β=7/3); isopiestic crystn. at 4°C gave the α-isomer; elem.anal.;
参考文献
Cambie, Richard C.; Clark, George R.; Gallagher, Stewart R.; Rutledge, Peter S.; Stone, Martin J.; Woodgate, Paul D.
Journal of Organometallic Chemistry, 1988 , vol. 342, p. 315 - 338
反应条件
in tetrahydrofuran; anhydrous butyl ether byproducts: C17H20O3; N2-atmosphere; refluxing ligand with 1.5 equiv. of Cr-complex (in Bu2O/THF=60:6.7) for 24 h; filtration (Celite), concn. (vac.), flash chromy. (hexanes/Et2O, then CH2Cl2); further unidentified Cr-complex; mixt. of isomers (α:β=2:3) not sepd., detd. by NMR spectroscopy; total yield 11percent;
参考文献
Clark, George R.; Kuipers, Bianca; Metzler, Michael R.; Nguyen, Manh H.; Woodgate, Paul D.
Journal of Organometallic Chemistry, 1997 , vol. 545-546, p. 225 - 247
反应条件
in decalin byproducts: CO; 3.5:1 mixture of arene and Cr(CO)6 in solvent purged for 20 min with Ar, evacuated for 20 min, mixture refluxed, cooled to 20°C, cooled to -18°C under argon, reaction time 3.5 h; filtered off, dissolved in benzene, filtered through Kieselguhr, concentrated, light petroleum added, crystn. at -18°C, complexes eluted with benzene/ethyl acetate, elem. anal., NMR;
参考文献
Hudecek, Milan; Toma, Stefan
Journal of Organometallic Chemistry, 1990 , vol. 393, # 1 p. 115 - 118
反应条件
in xylene byproducts: CO; Ar atmosphere, stirring, refluxing (145°C) overnight (14-16 h); xylenes removed in vac., residue dissolved in minimum volume CH2Cl2 and chromd. (silica gel, CH2Cl2); elem. anal.;
参考文献
Banse, Carolyn M.; Pray, Mellisa A.; Turnbull, Mark M.
Polyhedron, 1989 , vol. 8, p. 2719 - 2722
反应条件
acetic acid in decalin refluxing for 2.75 h;
参考文献
Hrnciar, Peter; Toma, Stefan
Journal of Organometallic Chemistry, 1991 , vol. 413, # 1-3 p. 161 - 164
反应条件
acetic acid in decalin refluxing for 3 h;
参考文献
Hrnciar, Peter; Toma, Stefan
Journal of Organometallic Chemistry, 1991 , vol. 413, # 1-3 p. 161 - 164
反应条件
in decalin refluxing for several hours;
参考文献
Hrnciar, Peter; Toma, Stefan
Journal of Organometallic Chemistry, 1991 , vol. 413, # 1-3 p. 161 - 164