二(甲基环戊二烯基)二氯化钛合成路线 (共 14 条)
反应条件
tetrahydrofuran; HCl in tetrahydrofuran; toluene under N2; addn. of anhydrous THF to a chilled toluene soln. of TiCl4 (-70°C), pptn. of TiCl4*2THF, temp. raised (-10°C), dropwise addn. of Na(C5H4Me) over 1 h, black suspn., stirred (1 d), treated with gaseous HCl, red suspn.; evapn. (to dryness), extn. (in air, CH2Cl2, Soxhlet), filtration, washed (Et2O, three times), evapn.; elem. anal.;
参考文献
Carofiglio, Tommaso; Floriani, Carlo; Sgamellotti, Antonio; Rosi, Marzio; Chiesi-Villa, Angiola; Rizzoli, Corrado
Journal of the Chemical Society, Dalton Transactions: Inorganic Chemistry (1972-1999), 1992 , # 6 p. 1081 - 1088
反应条件
in tetrahydrofuran byproducts: (C6H4OCH3PS)3; The soln. of reagents in THF was stirred for 20 h (N2 atm.);; evapd., recrystd. by dilution of CH2Cl2 soln. with methanol; elem. anal.;;
参考文献
Zank, Gregg A.; Rauchfuss, Thomas B.
Organometallics, 1984 , vol. 3, p. 1191 - 1199
反应条件
in carbon disulfide byproducts: Se; prevent light; added rapidly a soln. of CH3AsCl2 to a suspn. of Ti-complex at 0°C; detected by HPLC;
参考文献
Holz, Birger; Steudel, Ralf
Journal of Organometallic Chemistry, 1991 , vol. 406, # 1+2 p. 133 - 138
反应条件
in tetrahydrofuran byproducts: TlCl; stirring (30 min, pptn.); filtration, evapn. (vac.), recrystn. (CHCl3); elem. anal.;
参考文献
Chandra, Kailash; Sharma, R. K.; Garg, B. S.; Singh, R. P.
Inorganica Chimica Acta, 1979 , vol. 37, p. 125 - 128
反应条件
sodium in tetrahydrofuran dropwise addn. of 4 equiv. of sodium methylcyclopentadienide (prepd. from methylcyclopentadiene and Na) to TiCl4 at -20°C, stirring (roomtemp., overnight); solvent removal, dissoln. in CHCl3, filtration, solvent removal, drying (vac.), recrystn. (CHCl3); elem. anal.;
参考文献
Mokdsi, George; Harding, Margaret M.
Journal of Organometallic Chemistry, 1998 , vol. 565, # 1-2 p. 29 - 35
反应条件
in diethyl ether C5H4(CH3)Li slurry added slowly to TiCl4 soln. under Ar at 0°C, stirred for 30 min; evapd. (vac.), washed with aq. HCl, with EtOH, with ether, recrystd. (toluene), recrystd. (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 not given reaction was complete in 6 h at room temp.; no other products were formed; elem. anal. for Pt-complex;
参考文献
Giolando, Dean M.; Rauchfuss, Thomas B.; Clark, George M.
Inorganic Chemistry, 1987 , vol. 26, p. 3080 - 3082
反应条件
in dichloromethane exclusion of air, moisture, light; dropwise addn. of S2Cl2 in CH2Cl2 to Ti-complex in CH2Cl2 (0°C); vol. redn. (vac.), chromy. (Bio-Beads, CH2Cl2, >=15°C in the dark), evapn.;
参考文献
Steudel, Ralf; Westphal, Ursula
Journal of Organometallic Chemistry, 1990 , vol. 388, # 1+2 p. 89 - 94
反应条件
in not given reaction was complete in 6 h at room temp.; no other products were formed; elem. anal. for V-complex;
参考文献
Giolando, Dean M.; Rauchfuss, Thomas B.; Clark, George M.
Inorganic Chemistry, 1987 , vol. 26, p. 3080 - 3082
反应条件
in tetrachloromethane; toluene inert atmosphere, addn. of toluene/CCl4 soln. of COCl2 to a stirred CCl4 soln. of Ti complex at 0°C with exclusion of light, warming to 20°C with stirring (16 h); filtration (silica gel column, 15°C), extn. (THF), evapn. of solvent (vacuum), crystn. (-26°C, 20 h); elem. anal.;
参考文献
Steudel, Ralf; Westphal, Ursula; Pickardt, Joachim
Chemische Berichte, 1995 , vol. 128, # 6 p. 561 - 564