in benzene (N2); liquid BCl3 (46.0 mmol) condensed into soln. of the phenylene; mixt. allowed to warm to ambient temp.; 3 h stirring; (N2); solvent removed (vac.); residue distn. (50 °C, 1 mmHg);
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
in diethylene glycol dimethyl ether (N2); suspn. of NaBH4 (76.6 mmol) added to a stirred soln. of the o-phenyle compd. (51 mmol); B2H6 condensed at -196 °C (trap); after 1 h, mixt. heated to 90 °C for 90 min; (N2); pure B2H6 (condensed at -196 °C) obtained;
参考文献
Journal of the Chemical Society, Dalton Transactions: Inorganic Chemistry (1972-1999), , p. 1689 - 1692
LiCl in diethyl ether (N2); the phenylene compd. (0.53 mol) and NaBH4 (0.27 mol) allowed to react for 55 h in a steel ball mill after adding diethyl ether and LiCl; (N2); all volatiles were removed (vac.); fractional distn. of the condensate;
参考文献
Maennig, Detlef; Noeth, Heinrich
Journal of the Chemical Society, Dalton Transactions: Inorganic Chemistry (1972-1999), 1985 , p. 1689 - 1692
in tetrahydrofuran soln. of BH3*thf (120 mmol) in thf was added under N2 to 2,2'-o-phenylenedioxybis(1,3,2-benzodioxaborole) (120 mmol) which slowly dissolved on stirring; the react. was complete after 30 h (detected by (11)B-n.m.r. data);; the solvent was removed under vacuo (40-50 mm Hg) at ambient temp.; theconcd. soln. was then distd.;;
参考文献
Maennig, Detlef; Noeth, Heinrich
Journal of the Chemical Society, Dalton Transactions: Inorganic Chemistry (1972-1999), 1985 , 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
Maennig, Detlef; Noeth, Heinrich
Journal of the Chemical Society, Dalton Transactions: Inorganic Chemistry (1972-1999), 1985 , p. 1689 - 1692
in benzene 2,2'-o-phenylenedioxybis(1,3,2-benzodioxaborole) (115 mmol) was stirredunder N2 with H3B*SMe2 (115 mmol) for 12 d; benzene was then added and the mixt. stirred for 7 d;; monitored by (11)B n.m.r. expt.;;
参考文献
Maennig, Detlef; Noeth, Heinrich
Journal of the Chemical Society, Dalton Transactions: Inorganic Chemistry (1972-1999), 1985 , p. 1689 - 1692
