双茚基锆(VI)二氯化合物合成路线 （共 23 条）
反应条件
HCl in tetrahydrofuran N2 or Ar atmosphere; addn. of THF to ZrCl4 (-78°C), warming (room temp.), stirring (1 h), addn. of soln. of org. compd. in THF, stirring (1 h, room temp.), cooling (0°C), bubbling of HCl into soln.; partial evapn., addn. of Et2O, centrifugation, drying (vac.), sublimation (200-220°C, 0.03 mmHg); elem. anal.;
参考文献
Piccolrovazzi, Nicoletta; Pino, Piero; Consiglio, Gamgattista; Sironi, Angelo; Moret Massimo
Organometallics, 1990 , vol. 9, p. 3098 - 3105
反应条件
CH3Li in tetrahydrofuran; diethyl ether Ar, Schlenk technique; soln. of CH3Li in (C2H5)2O added dropwise at -80 °C to soln. of indene in THF, suspn. of ZrCl4 in cold THF added; solvents evapd. (vac.), residue washed ((C2H5)2O), extd. (CH2Cl2), extract evacuated to dryness, residue washed ((C2H5)2O, pentane), dried;
参考文献
Lapczuk-Krygier, Agnieszka; Baranowska, Katarzyna; Ponikiewski, Lukasz; Matern, Eberhard; Pikies, Jerzy
Inorganica Chimica Acta, 2012 , vol. 387, p. 361 - 365
反应条件
n-butyllithium in tetrahydrofuran; toluene treating indene in THF with n-C4H9Li in hexanes at -78°C, warming, stirring at room temp. for 1 h, cannulating the indenyllithium soln. into a suspension of ZrCl4*2THF in toluene at 0°C, warming, room temp. for 3 h; ppt., filtration, washing (THF/toluene, 1:2), sublimation (220°C, 1E-4 mmHg);
参考文献
Lee, Ik-Mo; Gauthier, William J.; Ball, JoAnne M.; Iyengar, Bhagavathi; Collins, Scott
Organometallics, 1992 , vol. 11, p. 2115 - 2122
反应条件
in dichloromethane-d2 (N2); Zr complex dissolved in CD2Cl2, CuCl added, stirred at room temp. for 6 h; CH2Cl2 added, filtered, dried;
参考文献
Balboni, Davide; Camurati, Isabella; Ingurgio, Antonio Cascio; Guidotti, Simona; Focante, Francesca; Resconi, Luigi
Journal of Organometallic Chemistry, 2003 , vol. 683, # 1 p. 2 - 10
反应条件
in toluene (N2); a soln. of SCl2 in toluene added to a suspn. of Zr complex in toluene, stirred for 45 min at room temp.; evapd. (vac.);
参考文献
Balboni, Davide; Camurati, Isabella; Ingurgio, Antonio Cascio; Guidotti, Simona; Focante, Francesca; Resconi, Luigi
Journal of Organometallic Chemistry, 2003 , vol. 683, # 1 p. 2 - 10
反应条件
in n-heptane; dichloromethane (N2); Zr complex dissolved in CH2Cl2, BCl3 in heptane added, stirred at room temp. for 1 h; dried;
参考文献
Balboni, Davide; Camurati, Isabella; Ingurgio, Antonio Cascio; Guidotti, Simona; Focante, Francesca; Resconi, Luigi
Journal of Organometallic Chemistry, 2003 , vol. 683, # 1 p. 2 - 10
反应条件
in diethyl ether; di-isopropyl ether; toluene (N2); a soln. of HCl in Et2O added to a soln. of Zr complex in toluene and iPr2O, stirred at room temp. for 2 h, evapd. (vac.), treated with ether, toluene and a soln. of HCl in Et2O, stirred for 2 h; evapd. (vac.);
参考文献
Balboni, Davide; Camurati, Isabella; Ingurgio, Antonio Cascio; Guidotti, Simona; Focante, Francesca; Resconi, Luigi
Journal of Organometallic Chemistry, 2003 , vol. 683, # 1 p. 2 - 10
反应条件
in n-heptane; dichloromethane (N2); indene dissolved in Et2O, MeLi/Et2O added with stirring at room temp., stirred for 40 min, a suspn. of ZrCl4 in pentane added, stirred at room temp. for 2 h, concd. (vac.), the powder slurried in CH2Cl2, BCl3 in heptane added at 0°C,; allowed to warm to room temp., stirred for 30 min, filtered, extd. with the same CH2Cl2 for 8 h, concd. (vac.); elem. anal.;
参考文献
Balboni, Davide; Camurati, Isabella; Ingurgio, Antonio Cascio; Guidotti, Simona; Focante, Francesca; Resconi, Luigi
Journal of Organometallic Chemistry, 2003 , vol. 683, # 1 p. 2 - 10
反应条件
in dichloromethane (N2); indene dissolved in Et2O, MeLi/Et2O added with stirring at room temp., stirred for 40 min, a suspn. of ZrCl4 in pentane added, stirred at room temp. for 2 h, concd. (vac.), the powder slurried in CH2Cl2, CuCl added, stirred for 3 h at room temp.; filtered, extd. with the same CH2Cl2 for 4 h, concd. (vac.), the powder slurried in pentane, filtered, dried (vac.);
参考文献
Balboni, Davide; Camurati, Isabella; Ingurgio, Antonio Cascio; Guidotti, Simona; Focante, Francesca; Resconi, Luigi
Journal of Organometallic Chemistry, 2003 , vol. 683, # 1 p. 2 - 10
反应条件
in diethyl ether; toluene byproducts: LiCl; (N2); a soln. of MeLi in Et2O added for 5 min at room temp. to a soln. of indene in Et2O, stirred for 30 min at room temp., added to a slurry ofZrCl4 in toluene, stirred for 80 min at room temp., filtered, treated a t room temp. with HCl soln. in Et2O,; stirred for 40 min at room temp., evapd. (vac.), washed with Et2O; elem.anal.;
参考文献
Balboni, Davide; Camurati, Isabella; Ingurgio, Antonio Cascio; Guidotti, Simona; Focante, Francesca; Resconi, Luigi
Journal of Organometallic Chemistry, 2003 , vol. 683, # 1 p. 2 - 10
