二(环戊二烯基)二氟钛(IV)合成路线 (共 18 条)
反应条件
in toluene (under dry N2 ); a suspn. of Me3SnF and of (C5Me5)TiCl3 in toluene is stirred at 80°C for 4 h; solvent is removed in vac., residue is sublimed at 130°C/0,01 mbar, elem. anal.;
参考文献
Herzog, Axel; Liu, Feng-Quan; Roesky, Herbert W.; Demsar, Alojz; Keller, Klaus; et al.
Organometallics, 1994 , vol. 13, p. 1251 - 1256
反应条件
in water absence of air; stoich. amts., stirring for 3 h; collection (filtration), drying overnight;
参考文献
Nath, Dina; Sharma, R. K.; Bhat, A. N.
Inorganica Chimica Acta, 1976 , vol. 20, p. 109 - 112
反应条件
hydrogen fluoride in not given refluxing Ti-complex with excess HF for 15 min; pptn. on cooling, filtration, drying (vac.);
参考文献
Nath, Dina; Sharma, R. K.; Bhat, A. N.
Inorganica Chimica Acta, 1976 , vol. 20, p. 109 - 112
反应条件
lithium tert-butylate in diethyl ether complex and lithium tert-butoxide dissolved in THF, stirred for 24 h atroom temp., solvent removed (vac.), extd. (petroleum ether), filtered (Ar), solvent removed (vac.), dissolved in ether, BF3*(C2H5)2O added slowly; ppt. washed with ether, dried (vac.), treated (MeOH), washed (ether), dried (vac.), sublimed at 120°C at 1E-6 Torr, recrystd. (hot toluene);
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 dichloromethane under Ar atm. Cp2TiCl2 was added to soln. triorganotin fluoride in CH2Cl2 and stirred for 3 h at 35°C; solvent was evapd. in vacuo, residue was washed with cold pentane and dried in vacuo;
参考文献
Bares, Josef; Novak, Petr; Nadvornik, Milan; Jambor, Roman; Lebl, Tomas; Cisarova, Ivana; Ruzicka, Ales; Holecek, Jaroslav
Organometallics, 2004 , vol. 23, # 12 p. 2967 - 2971
反应条件
pyridine or aniline in not given
参考文献
Bochmann, Manfred; Wilson, Ladislav M.; Hursthouse, Michael B.; Short, Richard L.
Organometallics, 1987 , vol. 6, p. 2556 - 2563
反应条件
in chloroform byproducts: CuCl; (N2); Schlenk technique; mixt. of Ti complex and Cu complex in CHCl3 wasstirred for 3 h; dried (vac.); residue extd. (CHCl3); filtered; filtrate dried (vac.); elem. anal.;
参考文献
Cauzzi, Daniele; Graiff, Claudia; Marazzi, Marianna; Predieri, Giovanni; Tiripicchio, Antonio
Journal of Organometallic Chemistry, 2002 , vol. 663, # 1-2 p. 256 - 262
反应条件
in tetrahydrofuran under N2; suspn. of Pd compd. in MeCN is added to a soln. of the Ti complex in THF, mixt. is stirred at room temp. overnight; solvent is removed, residue is washed with C6H6 and dried in vac., recrystd. from MeCN and benzene, solvent is removed from the benzene washings, the residue is washed with MeOH and identified as Cp2TiF2 by NMR; elem. anal.;
参考文献
Huang, Yujin; Drake, Robert J.; Stephan, Douglas W.
Inorganic Chemistry, 1993 , vol. 32, p. 3022 - 3028
反应条件
in acetone byproducts: silver bromide; addn. of AgBF4 soln. to Ti complex soln. (acetone), stirring (15 min); filtration, washing (acetone), addn. of Et2O to filtrate, cooling (-25°C), filtration, drying (vac.);
参考文献
Seyam, Afif; Samha, Hussein; Hodali, Hamdallah
Gazzetta Chimica Italiana, 1990 , vol. 120, p. 527 - 530
反应条件
in acetone byproducts: silver chloride; addn. of AgBF4 soln. to Ti complex soln. (acetone), stirring (15 min); filtration, washing (acetone), addn. of Et2O to filtrate, cooling (-25°C), filtration, drying (vac.);
参考文献
Seyam, Afif; Samha, Hussein; Hodali, Hamdallah
Gazzetta Chimica Italiana, 1990 , vol. 120, p. 527 - 530