hydrogenchloride in diethyl ether byproducts: LiCl, i-propanol; (N2); a soln. of B(O-i-Pr)3 cooled with a dry ice-acetone bath; CH3Li added slowly and stirred for 1 h; allowed to warm to room temp. with stirring for 3 h; cooled to 0°C; a soln. of HCl in ether added and stirred for 0.5 h; decanted; hydrolyzed with water; distd.; dried;
参考文献
Brown, Herbert C.; Cole, Thomas E.
Organometallics, 1985 , vol. 4, p. 816 - 821
in diethyl ether Schlenk techniques; titanocene dichloride in diethyl ether treated with2.23 equiv. of MeLi in diethyl ether at -40°C; stirred for 80 min with warming to 0°C; cooled to -40°C; water added; organic layer washed with water and brine; dried with MgSO4; evapd., recrystd. from pentane at -30°C;
in diethyl ether; toluene byproducts: LiCl; (N2); standard Schlenk technique; soln. of MeLi in ether was added to suspn. of Ti complex in toluene; mixt. was stirred at 0°C for 3 h; filtered; volatiles removed (vac.); residue redissolved in toluene; NMR monitoring;
in diethyl ether; benzene T=25°C; 1.5 h; ketone/MeLi ratio 1:2;
参考文献
Epsztajn, Jan; Bieniek, Adam
Journal of the Chemical Society, Perkin Transactions 1: Organic and Bio-Organic Chemistry (1972-1999), 1985 , p. 213 - 220