in diethyl ether React. of starting materials (NaBMe3H:BeCl2 = 2:1) in ether with stirring (30 min).; Filtn. and removal of solvent from filtrate under reduced pressure over 5-6 h leaves a white residue. Fractionation of volatile material yields Me3B. Elem. anal. of Be-compd.;
参考文献
Bell, Norman A.; Coates, Geoffrey E.; Heslop, J. Alan
Journal of Organometallic Chemistry, 1987 , vol. 329, # 3 p. 287 - 292
in tetrahydrofuran all operations performed under Ar or in vac., slight heating; evapn., mixture of at least 2 compds., Cp2TaCl2 identified by X-ray anal.;
in diethyl ether React. of starting materials (ether) in ratio NaBEt3H:BeCl2 = 2:1 results in immediate formation of a white ppt.; Removal of salt by filtn., evapn. of filtrate (room temp., reduced pressure), slow heating in vac. of remaining colourless oil and maintaining temp. at 90-100°C (12 h) gives a white solid. Fractionation yields Et3B. Elem. anal. of Be-compd.;
参考文献
Journal of Organometallic Chemistry, , vol. 329, # 3 p. 287 - 292
in neat (no solvent) Cp2Be was condensed into NMR tube on high vacuum line, then removed to N2 dry box for addition of BeCl2, to solids form viscous slush, after standing overnight LiSiMe3 was added, mixt. was heated; mixt. was condensed in dry C6D6; NMR;
参考文献
Saulys, Dovas A.; Powell, Douglas R.
Organometallics, 2003 , vol. 22, # 3 p. 407 - 413
C5H5Na in diethyl ether to soln. of freshly sublimed BeCl2 was added dropwise soln. of NaC5H5 and stirred for 3 h; solvent was removed and residue cooled (ice bath); product was sublimedthree times;
参考文献
Goddard, Richard; Akhtar, J.; Starowieyski, Kazimierz B.
Journal of Organometallic Chemistry, 1985 , vol. 282, p. 149 - 154
