双(异丙基环戊二烯)二氯化锆合成路线 (共 4 条)
反应条件
in hexane; toluene byproducts: C2H5CH=CH2; Ar-atmosphere; -78°C to 25°C (12 h), fulvene soln. (toluene addn., refluxing (8 h), filtering, washing (CHCl3), evapn. (vac.); chromy. (hexane / CHCl3);
参考文献
Eisch, John J.; Owuor, Fredrick A.; Shi, Xian
Organometallics, 1999 , vol. 18, # 9 p. 1583 - 1585
反应条件
in tetrahydrofuran addn. of ZrCl4 at 0°C to freshly prepared C5H4C3H7Li in THF withstirring 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
in hexane; toluene under Ar, 1.6 M hexane soln. of nBuLi was added to toluene soln. of ZrCl4 at -78 °C, warming to room temp., 6 h, fulvene-compd. was added, room temp. for 1 h and 65. degree.C for 6 h; mixt. was filtered, volatiles were removed in vac., extn. with hexane with a Soxhlet app. over 1 h;
参考文献
Eisch, John J.; Owuor, Fredrick A.; Shi, Xian
Polyhedron, 2005 , vol. 24, # 11 p. 1325 - 1339
反应条件
in toluene byproducts: (CH3)2SnCl2; (N2); using Schlenk techniques; addn. of Me2Sn(C5H4(i-Pr)-1)2 to ZrCl4 in toluene; 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