双(三甲基硅基环戊二烯)二氯化锆合成路线 (共 13 条)
反应条件
n-butyllithium in diethyl ether; hexane byproducts: n-butane, LiCl; addn. of soln. of n-butyllithium in hexane to soln. of isomeric mixture of cyclopentadiene derivative at -78 °C, addn. of ZrCl4 at -78 °C, stirred over night at room temp.; suspn. filtered of Na2SO4, evapn. in vac., washed with n-pentane, dried in vac;
参考文献
Journal of Organometallic Chemistry, , vol. 684, # 1-2 p. 91 - 104
反应条件
in benzene mixt. refluxed for 18 h; mixt. filtered; volatiles evapd.;
参考文献
Winter; Zhou; Dobbs; Heeg
Organometallics, 1991 , vol. 10, # 1 p. 210 - 214
反应条件
n-butyllithium in tetrahydrofuran Me3SiCl added slowly to NaCp at -78°C, warmed to room temp., recooled to -78°C, n-BuLi added dropwise, stirred for 30 min at roomtemp., recooled to 0°C, ZrCl4 in (CH3O)2CH2CH2 added dropwise, stirred overnight,; evapd. in vac., extd. in a Soxhlet apparatus with hexane, concd., filtered, recrystd. from boiling methylcyclohexane; elem. anal.;
参考文献
Siedle, A. R.; Newmark, R. A.; Lamanna, W. M.; Schroepfer, J. N.
Polyhedron, 1990 , vol. 9, p. 301 - 308
反应条件
in benzene refluxed for 10 h; volatiles evapd. under vac.; residue extd. with warm hexane, filtered; volatile evapd. under vac.;
参考文献
Organometallics, , vol. 10, # 1 p. 210 - 214
反应条件
Na in tetrahydrofuran 0.145 mmol of C5H5SiMe3 was added to a mixt. of sodium sand (130 mmol) and THF; after approx. 5 d the stirred soln. was cooled (0°C) and ZrCl4 (65 mmol) was added slowly over 0.5 h; the mixt. was stirred at 20°C for 2 h;; removal of THF in vacuo, followed by extn. with boiling hexane, filtration, concn. of the filtrate and cooling to -30°C;;
参考文献
Antinolo, Antonio; Lappert, Michael F.; Singh, Anirudh; Winterborn, Duncan J. W.; Engelhardt, Lutz M.; et al.
Journal of the Chemical Society, Dalton Transactions: Inorganic Chemistry (1972-1999), 1987 , p. 1463 - 1472
反应条件
in toluene byproducts: (CH3)2SnCl2; (N2); using Schlenk techniques; addn. of Me2Sn(C5H4SiMe3-1)2 to ZrCl4 intoluene; stirring under reflux for 24 h; evapn.; addn. of hexane; filtration, concn.; cooling; crystn., elem. anal.;
参考文献
Gomez-Ruiz, Santiago; Prashar, Sanjiv; Fajardo, Mariano; Antinolo, Antonio; Otero, Antonio
Journal of Organometallic Chemistry, 2007 , vol. 692, # 14 p. 3057 - 3064
反应条件
in tetrahydrofuran addn. of ZrCl4 at 0°C to freshly prepared C5H4Si(CH3)3Li in THF with stirring over 0.5 h, mixture stirred for further 24 h at 20°C; THF removed under vac., residue extd. with boiling toluene and little activated charcoal, filtered, addn. of hexane to filtrate, cooling to -30°C, elem. anal.;
参考文献
Lappert, Michael F.; Pickett, Christopher J.; Riely, Paul I.; Yarrow, Paul I. W.
Journal of the Chemical Society, Dalton Transactions: Inorganic Chemistry (1972-1999), 1981 , p. 805 - 813
反应条件
aq. HCl in diethyl ether byproducts: HO(CH2)2C.tplbond.CH; N2-atmosphere; 25°C;
参考文献
Journal of Organometallic Chemistry, , vol. 524, # 1-2 p. 49 - 61
反应条件
aq. HCl in diethyl ether byproducts: HO(CH2)2C.tplbond.CH; N2-atmosphere; 25°C;
参考文献
Journal of Organometallic Chemistry, , vol. 524, # 1-2 p. 49 - 61
反应条件
aq. HCl in dichloromethane N2-atmosphere; 25°C;
参考文献
Journal of Organometallic Chemistry, , vol. 524, # 1-2 p. 49 - 61