in further solvent(s) soln. NaBH4 in triglyme (tetraglyme) was added slowly for 2-3 h at roomtemp. to NaBF4 and AlCl3 in triglyme (tetraglyme); B2H6 was absorbed with THF;
in diethylene glycol dimethyl ether to a soln. of NaBH4 (22.2 mmol) in diglyme was added dropwise with stirring under N2 a soln. of catecholatoborane (44.4 mmol) in diglyme; B2H6 was absorbed in acetone (for 16 h);; after evapn. of the solvent the solid residue was dried at 100°C(1E-2 mm Hg);;
参考文献
Journal of the Chemical Society, Dalton Transactions: Inorganic Chemistry (1972-1999), , p. 1689 - 1692
in diethylene glycol dimethyl ether (N2); soln. of Na(BH4) (34.1 mmol) in diglyme was added to the phenylene compd. (68.3 mmol) in diglyme; B2H6 carried away by an N2 stream, was absorbed in acetone; stirring overnight; (N2); distn. (80-100 °C, 100 mmHg) gave a soln. of the catecholatoborane (yield 97percent); the non-volatile residue dried (100 °C, 0.01 mmHg) and identfied as Na(B(O2C6H4)2) (11B NMR spectrum);
参考文献
Journal of the Chemical Society, Dalton Transactions: Inorganic Chemistry (1972-1999), , p. 1689 - 1692
