1,2-双(二甲基瞵)乙烷合成路线 (共 25 条)
反应条件
in tetrahydrofuran; ethylene glycol dimethyl ether soln. of Ti(CO)3(dmpe)2 in DME stirred under CO for 3 h and then cooled to 0°C; cooled soln. of Na(DME)C5H5 in THF added; mixt. warmed to room temp.; CO replaced by Ar atmosphere; addn. of Et4NBr; filtration, removal of solvents and dmpe in vac.; cryst. product washed with ethanol (0°C) and dried in vac.;
参考文献
Chi,K.M.; Frerichs,S.R.; Kelseystein,B.
Journal of the American Chemical Society, 1988 , vol. 110, p. 163
反应条件
in ethylene glycol dimethyl ether soln. of Ti(CO)3(dmpe)2 in DME stirred under CO at room temp. for 3 h; addn. of Na(DME)(C9H7) in DME at -30°C; soln. slowly warmed to room temp. over a period of 12 h; addn. of Et4NBr; slurry stirred for further 12 h; filtration, redn. of vol., addn. of diethyl ether; ppt. washed with ether and dried in vac.;
参考文献
Chi,K.M.; Frerichs,S.R.; Kelseystein,B.
Journal of the American Chemical Society, 1988 , vol. 110, p. 163
反应条件
in benzene (C5Me5)Ru(NO)Ph2 was heated with 1,2-bis(dimethylphosphino)ethane and benzene in vacuum at 45 °C for 45 h;; the volatile materials were removed in vacuum, the residue was purified by crystn. from toluene layered with an equal portion of pentane at -40 °C; elem. anal.;;
参考文献
Chang,J.; Bergman,R.G.
Journal of the American Chemical Society, 1987 , vol. 109, p. 4298
参考文献
Maeding, Peter
Zeitschrift fuer Chemie (Stuttgart, Germany), 1986 , vol. 26, # 11 p. 408 - 409
反应条件
in ethylene glycol dimethyl ether soln. of Ti(CO)3(dmpe)2 in DME stirred under CO for 3 h; addn. of K(HBpz3) in DME; after 3 h addn. of Et4NBr; stirring continued for 6 h; filtration, solvent removed in vac. at room temp.; resulting solid washed with toluene, ethanol, and ether; recrystn. from acetonitrile/toluene; elem. anal.;
参考文献
Chi,K.M.; Frerichs,S.R.; Kelseystein,B.
Journal of the American Chemical Society, 1988 , vol. 110, p. 163
反应条件
in diethyl ether Satn. of an ether soln. of CpZr(dmpe)2Cl with butadiene (N2, room temp., 1 atm).; Separation of cryst. CpZr(η4-butadiene)(dmpe)Cl after changing of color.;
参考文献
Wielstra, Ytsen; Gambarotta, Sandro; Roedelof, Johannes B.
Organometallics, 1988 , vol. 7, p. 2177 - 2182
反应条件
in diethyl ether byproducts: methane; react. with 3 equiv. of ethylene at room temp. and atmospheric pressure; recrystn.;
参考文献
Wielstra, Ytsen; Gambarotta, Sandro; Chiang, Michael Y.
Organometallics, 1988 , vol. 7, p. 1866 - 1867
反应条件
in benzene byproducts: CH4, C2H6, C2H4 or C2H2; thermal decomposition at 90°C;
参考文献
Organometallics, , vol. 8, p. 2907 - 2917
反应条件
in benzene-d6 (N2); pressurizing of Zr-complex with butadiene; not isolated; NMR spectroscopic monitoring;
参考文献
Wielstra, Ytsen; Gambarotta, Sandro; Spek, Anthony L.
Organometallics, 1990 , vol. 9, p. 572 - 577
反应条件
bis(cyclopentadienyl)titanium dichloride
参考文献
Phosphorus, Sulfur and Silicon and the Related Elements, , vol. 77, # 1-4 p. 41 - 44