双(叔丁基环戊二烯)二氯化钛合成路线 (共 3 条)
反应条件
sodium in tetrahydrofuran; benzene byproducts: NaCl; to metallic Na in THF t-BuC5H5 added at -20°C; after 2 h n-BuCl in THF added dropwise; stirred for 10 h; NaCl filtered off; TiCl4 in THF/benzene added at 0°C to the filtrate; stirred for 3 h at -20°C; satd. with dry HCl; solvent evapd. in vacuo; residue extd. (HCl-satd. CHCl3); recrystd. (CHCl3); elem. anal.;
参考文献
Strelets, V. V.; Soloveichik, G. L.; Sizov, A. I.; Bulichev, B. M.; Rusina, A.; Vlchek, A. A.
Bulletin of the Academy of Sciences of the USSR, Division of Chemical Science (English Translation), 1983 , vol. 32, p. 2241 - 2245
Izvestiya Akademii Nauk SSSR, Seriya Khimicheskaya, 1983 , p. 2493 - 2497
反应条件
in tetrahydrofuran under Ar, addn. of TiCl4 to a THF soln. at 0°C, dropwise addn. of (C5H4CMe3)Li in THF, allowed to warm to room temp., stirred for 2 h; addn. of heptane, pptn. filtered off in air, recrystn. (CHCl3);
参考文献
Martin, J.; Fauconet, M.; Moise, C.
Journal of Organometallic Chemistry, 1989 , vol. 371, p. 87 - 100
反应条件
in tetrahydrofuran adding ((tBuCp)2TiCl)2 in THF to freshly sublimated S8 under stirring at room temp. , react. time: 3d , argon atmosphere; equil.; flash chromatography, elem. anal.;
参考文献
Phosphorus and Sulfur and the Related Elements, , vol. 36, p. 11 - 14