双(五甲基环戊烯)二氯化钛合成路线 (共 24 条)
反应条件
samarium diiodide in tetrahydrofuran reaction at -35°C (1 h), warming to 40°C;
参考文献
Casty, Gary L.; Stryker, Jeffrey M.
Journal of the American Chemical Society, 1995 , vol. 117, # 29 p. 7814 - 7815
反应条件
samarium diiodide in tetrahydrofuran reaction at -35°C (0.7 h), warming to 40°C;
参考文献
Casty, Gary L.; Stryker, Jeffrey M.
Journal of the American Chemical Society, 1995 , vol. 117, # 29 p. 7814 - 7815
反应条件
samarium diiodide in tetrahydrofuran reaction at -35°C (5 h), warming to 40°C;
参考文献
Casty, Gary L.; Stryker, Jeffrey M.
Journal of the American Chemical Society, 1995 , vol. 117, # 29 p. 7814 - 7815
反应条件
samarium diiodide in tetrahydrofuran reaction at -35°C (2 h), warming to 40°C;
参考文献
Casty, Gary L.; Stryker, Jeffrey M.
Journal of the American Chemical Society, 1995 , vol. 117, # 29 p. 7814 - 7815
反应条件
air in ethanol; benzene byproducts: CO2; Ar-atmosphere; freezing soln. of Ti-complex (in C6H6), mixing with 6.5 NHCl (in EtOH); evapn. (vac.), extn. into CHCl3 in air, evapn. (vac.);
参考文献
Burlakov; Dolgushin; Yanovsky; Struchkov; Shur; Rosenthal; Thewalt
Journal of Organometallic Chemistry, 1996 , vol. 522, # 2 p. 241 - 247
反应条件
in tetrahydrofuran 0.5 equiv. of PbCl2, 20°C;
参考文献
Journal of the American Chemical Society, , vol. 117, # 29 p. 7814 - 7815
反应条件
HCl in toluene (Ar), HCl gas (1 atm static pressure) added to a soln. of the complex, stirred for 1 h; excess HCl pumped away, toluene removed under vacuum, hexane added, stirred for a few minutes, filtered, (C5(CH3)5)2TiCl2 pptd., filtrate evapd. under vacuum, (C5(CH3)5)TiCl3 crystd., elem. anal.;
参考文献
Organometallics, , vol. 4, p. 550 - 553
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 tetrahydrofuran reaction at -35°C (4 h), warming to room temp.;
参考文献
Journal of the American Chemical Society, , vol. 117, # 29 p. 7814 - 7815
反应条件
CH3CH2CH2CH2Li in tetrahydrofuran byproducts: LiCl; Ar; TiCL3 solution was added to a slurry containing 2.2 equ. of CpLi; 24 h reflux; the reaction mixture was poured into 2N HCl;; the product separated as crystals; the mother liquor was extracted with CHCl3, the organic phase was dried and evaporated to dryness; crystn. from CHCl3/CH3OH; the purity was checked by mass spectrometry;;
参考文献
Journal of Organometallic Chemistry, , vol. 333, p. 205 - 216