in dichloromethane-d2 Kinetics; byproducts: (CH3)3COH; (Ar or N2); keeping a soln. of titanium complex in CD2Cl2 at 283-313 K; not isolated, detected by NMR;
参考文献
DiPasquale, Antonio G.; Hrovat, David A.; Mayer, James M.
Organometallics, 2006 , vol. 25, # 4 p. 915 - 924
in tetrahydrofuran under Ar using Schlenk techniques; soln. of Ti(N(Ph)CH2CH2C5H4N)Cl3 in THF cooled to -95°C; soln. of NaC5H5 in THF added dropwise; mixt. stirred for 5.5 h; slowly warmed to room temp.; volatiles removed; residue extd. (toluene); soln. concd. and placed at -20°C; elem. anal;
参考文献
Ascenso, Jose R.; De Azevedo, Cristina G.; Dias, Alberto R.; Duarte, M. Teresa; Eleuterio, Ines; Ferreira, Maria Joao; Gomes, Pedro T.; Martins, Ana M.
Journal of Organometallic Chemistry, 2001 , vol. 632, # 1-2 p. 17 - 26
in toluene byproducts: bis[tris(trimethylsilyl)hydrazino]P2Cl2, bis(trimethylsilyl)acetylene; using Schlenk techniques; dissolving of Cp2Ti(Me3SiC)2 (2 mmol) in toluene at -78°C; addn. of (tris(trimethylsilyl)hydrazino)PCl2 (4 mmol) by syringe; stirring for 15 min; warming to room temp.; stepwise removal of solvent; cooling to -40°C; crystn.;
in tetrahydrofuran Li compd. in THF added slowly to complex soln. under Ar at room temp., stirred for 30 min; evapd. (vac.), washed with aq. HCl, with EtOH, with ether, recrystd. (hot CHCl3 or toluene);
参考文献
Ott, Kevin C.; deBoer, E. J. M.; Grubbs, Robert H.
Organometallics, 1984 , vol. 3, p. 223 - 230
in hexadeuterioacetone to cold (-78 °C) soln. of Ti complex in acetone-d6 added soln. of HgCl2 in acetone-d6 under N2 (1:1 molar ratio); warmed to room temp., monitored by NMR;
in carbon disulfide SeCl2 is added to the sulfide within 1 min, the mixture is stirred for 7 min; the TiCl2-compd. is sucked, the residue is dissolved in CS2 at 20°C, the undissolved residue is filtered off, the soln. is allowed to flow into cold pentane, crystals are washed with cold n-pentane and dried in vacuum at -78°C for 2 h;
in deuterated toluene stirring of the combined solns. under Ar; flask fitted with a closed valve; further product: intractable black ppt. (Rh(x)(CO)y or Pd); not isolated; monitored by 1H NMR;
in toluene byproducts: P(CH3)3; dry solvents; addn. of acetyl chloride to Ti-compd. dropwise at room temperature, stirring (1 h) at room temperature; filtration, concn., layering with pentane, crystn. and pptn. by storing soln. at -50°C; detn. by (1)H-NMR and IR spectroscopy;
