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首页> 外文期刊>Zeitschrift fur Anorganische und Allgemeine Chemie >PREPARATION AND SPECTROSCOPIC CHARACTERIZATION OF CARBOXYLATODODECABORATES [German]
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PREPARATION AND SPECTROSCOPIC CHARACTERIZATION OF CARBOXYLATODODECABORATES [German]

机译:羧十二碳酸盐的制备和光谱表征[德语]

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摘要

The tetrabutylammonium salt (TBA)(2)[B12H12](2-) reacts with formic, acetic, cyanoacetic, phenylacetic, propionic, butyric, and thioacetic acid at temperatures between 80 and 150 degrees C forming the carboxylatododecaborates [(RC(O)O)(n)-B12H12-n](2-), n = 1, 2, [CH3C(O)S-B12H11](2-). The isolation of the pure compounds is achieved by ion exchange chromatography on diethylaminoethyl cellulose. In case of the dicarboxylatododecaborates beside the 1,7-isomer predominantly the 1,2-isomer, while 1,2-[(OH)C6H5CH2C(O)O-B12H10](2-) is formed exclusively. The alcaline hydrolysis of [RC(O)O-B12H11](2-) and 1,2[(OH)C6H5CH2C(O)O-B12H10](2-) results in [(OH)-B12H11](2-) and 1,2-[(OH)(2)-B12H10](2-). All compounds are characterized by their B-11-nmr, C-13-nmr and IR spectra. The B-11-nmr signals are assigned by a sheme allowing to establish expected spectra. [References: 16]
机译:四丁基铵盐(TBA)(2)[B12H12](2-)在80至150摄氏度的温度下与甲酸,乙酸,氰基乙酸,苯乙酸,丙酸,丁酸和硫代乙酸反应,形成羧基十二碳六硼酸盐[[RC(O) O)(n)-B 12 H 12 -n](2-),n = 1、2,[CH 3 C(O)S-B 12 H 11](2-)。通过在二乙基氨基乙基纤维素上的离子交换色谱法来分离纯净的化合物。在除1,7-异构体外主要是1,2-异构体的情况下,二羧基latododecaboates,而仅形成1,2-[(OH)C6H5CH2C(O)O-B12H10](2-)。 [RC(O)O-B12H11](2-)和1,2 [(OH)C6H5CH2C(O)O-B12H10](2-)的碱水解产生[(OH)-B12H11](2-)和1,2-[(OH)(2)-B12H10](2-)。所有化合物均以其B-11-nmr,C-13-nmr和IR光谱为特征。 B-11-nmr信号由Sheme分配,从而可以建立预期的光谱。 [参考:16]

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