双(五甲基环戊二烯)二甲基锆合成路线 （共 12 条）
反应条件
in diethyl ether byproducts: LiCl; MeLi (Et2O) is added to (C5Me5)2ZrCl2 (Et2O) under Ar, mixt. is stirred for 6 h.; Evapn., extn. (petroleum ether), concg. yields ppt., cooling to -78°C, filtn.;
参考文献
Miller, Frederick D.; Sanner, Robert D.
Organometallics, 1988 , vol. 7, p. 818 - 825
反应条件
in toluene N2-atmosphere; room temp. (5 h); evapn. (vac.), recrystn. (n-hexane, -25°C), filtering, drying (vac.); elem. anal.;
参考文献
Herzog, Axel; Roesky, Herbert W.; Jaeger, Felix; Steiner, Alexander; Noltemeyer, Mathias
Organometallics, 1996 , vol. 15, # 3 p. 909 - 917
反应条件
in dichloromethane-d2 Al/Zr=2-8, reacted in NMR tube; not isolated, detected by NMR;
参考文献
Journal of Molecular Catalysis A: Chemical, , vol. 210, # 1-2 p. 47 - 52
反应条件
in dichloromethane not isolated; monitored by 13C NMR;
参考文献
Polyhedron, , vol. 9, p. 301 - 308
反应条件
in deuterated toluene using Schlenk techniques; mixing of solns. of B(C6F5)3 and Al2Me6 in toluene-d8 in NMR tube for 10 min, addn. of soln. of ZrMe2(C5Me5)2 in toluene-d8 at 20°C with ratio B(C6F5)3, Al2Me6 and (C5Me5)2ZrMe2 1:2:1; monitoring by NMR;
参考文献
Mathis, Deborah; Couzijn, Erik P. A.; Chen, Peter
Organometallics, 2011 , vol. 30, # 14 p. 3834 - 3843
反应条件
CO in dichloromethane-d2 charging a NMR tube containing Zr-complex, B(C6F5)3 and CD2Cl2 with 1 atm of CO at 23°C, mixing for 5 min; monitoring by (1)H-NMR; mixt. of 75percent carbonyl complex and 25percent dichloro complex; further not identified ((CH3)5C5)2Zr species in soln.; removal of solvent in vacuo;
参考文献
Organometallics, , vol. 13, p. 766 - 773
反应条件
in dichloromethane-d2 charging a NMR tube containing Zr-complex and CD2Cl2 with 1 atm of (13)CO at 23°C, mixing for 5 min; monitoring by (1)H-NMR, removal of solvent in vacuo;
参考文献
Organometallics, , vol. 13, p. 766 - 773
反应条件
in deuterated toluene byproducts: Al(C6F5)3; using Schlenk techniques; mixing of solns. of B(C6F5)3 and Al2Me6 in toluene-d8 in NMR tube for 10 min, addn. of soln. of ZrMe2(C5Me5)2 in toluene-d8 at 20°C with ratio B(C6F5)3, Al2Me6 and (C5Me5)2ZrMe2 2:1:1; monitoring by NMR;
参考文献
Mathis, Deborah; Couzijn, Erik P. A.; Chen, Peter
Organometallics, 2011 , vol. 30, # 14 p. 3834 - 3843
反应条件
in methylcyclohexane-d14
参考文献
Colorado State University Research Foundation
Patent: US6335466 B1, 2002 ;
Location in patent: Example 28 ;
反应条件
in methycyclohexane-d14
T=70°C; 1 h;
参考文献
Colorado State University Research Foundation
Patent: US6335466 B1, 2002 ;
Location in patent: Example 28 ;
