catalyst: dioxane-d8 in 1,4-dioxane-d8; perdeuterocyclohexane Kinetics; Cr-complex was heated in C6D12 in the presence of dioxane-d8 (4.0 M) at 170°C; rate consts. for external arene exchange are given; (1)H NMR analysis of reaction mixt.;
cesium fluoride in N,N-dimethyl-formamide addn. of Cr complex to CsF under N2, 20°C; successive dropwise addn. of DMF and aldehyde via syringe; addn. of diethyl ether; reacting, 6h; filtration; washing filtrate (H2O); drying (K2SO4); evapn. to dryness; fractionated crystn. (n-hexane); elem. anal.;
cesium fluoride in N,N-dimethyl-formamide stirring at room temp. for 6.0 h in inert atm.; washed with water, diluted with ether, filtered, dried with Na2SO4, crystd. in n-hexane;
in tetrahydrofuran; anhydrous butyl ether (under N2); ratio aryl-compd.:Cr(CO)6 1:1, reflux for 67 h in Bu2O-THF; removal of the solvents, sublimation of the residue;
参考文献
Beckett, Michael A.; Gilmore, Robert J.; Idrees, Khalid
Journal of Organometallic Chemistry, 1993 , vol. 455, # 1-2 p. 47 - 49
Fischer, E. O.; Oefele, K.
Angewandte Chemie, 1957 , vol. 69, p. 715 - 715
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Gmelin Handbook: Cr: Org.Verb., 1.6.1.2.1.1, page 183 - 190
benzene in tetrahydrofuran heating educt in THF in presence of 10-fold excess of both benzene and cycloheptatriene in sealed tubes (90°C for 14 days, or 135°C for 20 h);
参考文献
Hoff, Carl D.
Journal of Organometallic Chemistry, 1983 , vol. 246, # 2 p. C53 - C56
benzene in benzene Kinetics; in silylated (5percent CH3C(OSiMe3)=NSiMe3 in ether) NMR tube, under nitrogen atmosphere; haptotropic rearrangement was monitored by (2)H NMR spectroscopy at 60, 70, 80, and 87°C;