HCl in tetrahydrofuran byproducts: NaCl; under Ar; to the Ga-compd. (generated in situ from Ga(CH2CMe3)2Cl and Na/C10H8 in THF at -78°C) was added anhyd. HCl, soln. became colorless; volatile components removed (vacuum distn.), liq. subjected to a dynamic vacuum for 18 h, solid dissolved in pentane, insol. portion (NaCl) repeatedly washed;

1: Na/naphthalene / tetrahydrofuran 2: HCl / tetrahydrofuran View Scheme

sodium in neat (no solvent) Ar-atmosphere; stirring (-70°C, 1 h); evapn., extg. (pentane); elem. anal.;

Na/naphthalene in tetrahydrofuran byproducts: NaCl; under Ar; Ga-compd./THF added slowly to Na naphthalenide/THF at room temp. over 30 min, mixt. stirred; THF removed (rapid vacuum distn.), mixt. subjected to dynamic vac. (24 h), volatile materials trapped (Ga(CH3CMe3)3 and C10H8); non-volatile residue extd. (pentane), filtered, evapn.; elem. anal.;

Na; C10H8 in tetrahydrofuran byproducts: NaCl, C10H10, C10H8; Ar-atmosphere; stirring (room temp., 5 d); evapn. (vac.), drying (dynamic vac., 24 h), extg. (pentane), recrystn. (-78°C); elem. anal.;