名称:
Reaction of B11H14NR4 (REt, Bu) with M2O3 (MAs, Sb, Bi) in biphasic systems
摘要:
The reaction of B11H14NR4 (R = Et, Bu) with M2O3 (M = As, Sb Bi) in biphasic systems H2O/CH2Cl2 or NaOH/CH2Cl2, with C6H5NEt3Cl as phase transfer catalyst, was investigated as a new route to the already described icosahedral B11H11MNR4 (M = As, Sb, Bi; R = Et, Bu). When the above reaction was performed in basic medium, besides the expected heteroboranes, a new anionic species could be isolated and characterized by its 1D B-11, H-1{B-11} and 2D B-11-B-11 NMR spectra. Consistently with these data the formula B11H13OB11H13 2-,2NEt4+ is proposed, the anionic part consisting of two icosahedral fragments B11H13 (eleven normal B-H bonds and two bridge hydrogens in the open face) linked via a B-O-B bond; on both sides, the oxygen atom is attached, in endo position, to the unbridged boron atom of the open face. The same compound could be prepared by reaction of B11H14- with PO4HNa2, in NaOH/CH2Cl2 mixtures. A possible path involving a mild oxidation of B11H13(2-) by M2O3 (M = As, Sb, Bi) is suggested.