in tetrahydrofuran byproducts: Li-phthalate; under N2, Li-salt ws dissolved at -78 °C in THF, B-compd. in THF was added, several h; using 3 equiv. of solid alkali-compd. gave reproducible results; solvent was removed in vac., washing with Et2O and dissolving in THF, storage at -20 °C when B(NMePh)3 was formed; Li-complex was detected only in soln. by (11)B NMR;

in tetrahydrofuran byproducts: Na-phthalate; under N2, B-compd. in THF was added to THF soln. of Na-compd., solvent was removed, extd. with hexane and Et2O; using 3 equiv. of solid alkali-compd. gave reproducible result; monitored by (11)B NMR; hexane phase was crystd. for 2 weeks at -80 °C which lead to the solvated compd., Et2O contained NaB(OtBu)4, the hexane phase contained HB(OtBu)2 and B(OtBu)3;