(五甲基环戊二烯基)三氯化钛(IV)合成路线 （共 17 条）
反应条件
in not given room temp.;
参考文献
Scherer, Otto J.; Swarowsky, Herbert; Wolmershaeuser, Gotthelf; Kaim, Wolfgang; Kohlmann, Stephan
Angewandte Chemie, 1987 , vol. 99, p. 1178 - 1179
反应条件
140 ° C; 4h; equimolar amounts;; the product was twice sublimed in vacuo; the purity was checked by mass spectrometry;;
参考文献
Journal of Organometallic Chemistry, , vol. 333, p. 205 - 216
反应条件
in tetrahydrofuran addn. of the Ti compd. to the Tl compd. in THF in an Ar-flushed Schlenk flask and stirring for 19 h; filtn. through a celite plug on a glas frit, evapn., extn. of the residue in a Soxhlet with hexane (10 h) and CCl4 (12 h), evapn. and crystn. from CH2Cl2-hexane; elem. anal.;
参考文献
Rausch, Marvin D.; Spink, W. Craig
Synthesis and Reactivity in Inorganic and Metal-Organic Chemistry, 1989 , vol. 19, p. 1093 - 1102
反应条件
magnesium in tetrahydrofuran N2 atmosphere; Mg stirring (24 h, room temp.); solvent removal (vac.), extn. (pentane), recrystn. (pentane), sublimation (100 - 150°C, 0.1 mm Hg); elem. anal.;
参考文献
Blenkers, J.; Bruin, P.; Teuben, J. H.
Journal of Organometallic Chemistry, 1985 , vol. 297, p. 61 - 68
反应条件
in tetrahydrofuran Ar-atmosphere; dropwise addn. of K2C8H8 to Ti-complex (during 30 min), stirring (room temp., 90 min), refluxing (15 min); solvent removal (reduced pressure), sublimation (120°C/0.2 Torr); elem. anal.;
参考文献
Kool, Larry B.; Rausch, Marvin D.; Rogers, Robin D.
Journal of Organometallic Chemistry, 1985 , vol. 297, p. 289 - 300
反应条件
in tetrahydrofuran C5H5Li suspn. added slowly to stirred complex soln. under Ar at ambienttemp., stirred for 30 min; evapd. (vac.), washed with aq. HCl, with EtOH, with ether, recrystd. (hot toluene, CHCl3);
参考文献
Ott, Kevin C.; deBoer, E. J. M.; Grubbs, Robert H.
Organometallics, 1984 , vol. 3, p. 223 - 230
反应条件
in diethyl ether; hexane byproducts: LiCl; all manipulations carried out under dry Ar; soln. of LiMe in diethyl ether slowly added to an ice-cold suspension of Ti-compd. in hexane, mixt. left to reach room temp. with stirring for 4h; filtered, evapd., recrystn. (pentane, -78°C); elem. anal.;
参考文献
Mena, Miguel; Royo, Pascual; Serrano, Ricardo; Pellinghelli, Maria Angela; Tiripicchio, Antonio
Organometallics, 1989 , vol. 8, p. 476 - 482
