in pentane byproducts: NaCl; all manipulations with exclusion of air and moisture; excess of soln. ofNa compd. added dropwise to cooled soln. of GaCl3 (-30°C); controlled by NMR; volatiles evapd. by oil pump, residue dissolved in pentane, NaCl filtered, filtrate concd., product crystd. at -23°C; elem. anal.;

in pentane byproducts: NaCl; (inert conditions); removal of volatiles (vac.), addn. of pentane, filtration, evapn.;

in pentane byproducts: NaCl, NaSi(t-Bu)3; dropwise addn. of 1 equiv. Si-compd. to GaCl3 at room temp.; removal of volatiles, pentane addn., filtration off of NaCl, crystn. (-23°C, 12 h); elem. anal.;

in pentane byproducts: NaCl; (inert conditions); removal of volatiles (vac.), addn. of pentane, filtration, crystn. on concn.; elem. anal.;

in pentane byproducts: NaCl; all manipulations with exclusion of air and moisture; soln. of Na compd.added dropwise to cooled soln. of GaCl3 (-30°C) in molar ratio o f 1:1; react. mixt. contained second and main product in molar ratio of 1:4 - controlled by NMR; volatiles evapd. by oil pump, residue dissolved in pentane, NaCl filtered, filtrate concd., product crystd. at -23°C; elem. anal.;

in tetrachloromethane; pentane byproducts: (t-Bu)3SiH, (t-Bu)3SiCl; Cl2 in CCl4 was reacted with Ga-compd. in pentane at -78 °C; unidentified products were also formed;

in pentane byproducts: NaCl, [Si(t-Bu)3]2; dropwise addn. of 3 equiv. Si-compd. to GaCl3 at -30°C, warming to room temp.; removal of volatiles, pentane addn., filtration off of NaCl, vol. reduction, fractional crystn. (-23°C, 5 d);

in pentane 2 equiv. Si-compd.; removal of volatiles, pentane addn., filtration off of NaCl, crystn.;

1: n-heptane 2: not given View Scheme

1: n-heptane 2: benzene-d6 View Scheme