benzene in benzene
Sonication; TiCl4 under Ar dissolved in benzene is immersed in an ultrasonic bath for 60 min at room temp., addn. of K(BEt3H) in benzene, for 60 min in the ultrasonic bath; filtn. of the ppt., washing (benzene), removal the solvent of the filtrate, dissolving the residue in pentane, filtn., removal the pentane, recrystn. of the residue (pentane);
in solid matrix
condensation of vaporized Ti in high vac. with solid benzene matrix cooled with liq. N2;
参考文献
Kvashina, E. F.; Petrova, G. N.; Belov, G. P.; Roshchupkina, O. S.; Efimov, O. N.
Russian Chemical Bulletin, 2002 , vol. 51, # 5 p. 817 - 819
Izvestiya Akademi Nauk, Seriya Khimicheskaya, 2002 , vol. 51, # 5 p. 754 - 756
benzene in benzene
absence of air and moisture; co-condensing Ti-vapour (obtained by resistance heating of 85percent Ti - 15percent Mo alloy) with equimolar amt. of C7H8 and excess of C6H6 vapours, warming to room temp.; evacuation, extn. into hexane, crystn. (-78°C); product mixt. (cycloheptatriene:benzene complex = 1.2:1.0) not sepd., detd. by (1)H-NMR spectroscopy;
参考文献
Timms, Peter L.; Turney, Terence W.
Journal of the Chemical Society, Dalton Transactions: Inorganic Chemistry (1972-1999), 1976 , p. 2021 - 2025
in neat (no solvent, gas phase)
prepn. by laser evapn. of Ti atom from metal rod; evaporized atoms were cooled down by collisions with He carrier gas; C6H6 vapor mixed followedby the size and structure selection with 2-m long electrostatic hexapol e field;
参考文献
Imura, Kohei; Ohoyama, Hiroshi; Kasai, Toshio
Chemical Physics, 2004 , vol. 301, # 2-3 p. 183 - 187