Křížková Adéla, Bastien Guillaume, Rončević Igor, Císařová Ivana, Rybáček Jiří, Kašička Václav, Kaleta Jiří
Institute of Organic Chemistry and Biochemistry of the Czech Academy of Sciences, Flemingovo nám. 2, 160 00 Prague 6, Czech Republic.
Department of Inorganic Chemistry, Faculty of Science, Charles University in Prague, Hlavova 2030, 128 40 Prague 2, Czech Republic.
J Org Chem. 2024 Aug 16;89(16):11100-11108. doi: 10.1021/acs.joc.2c02872. Epub 2023 Feb 1.
Herein, we report radical chlorination of cubane-1,4-dicarboxylic acid leading preferentially to one monochlorinated cubane dicarboxylate (ca. 70%) that is accompanied by four dichlorinated derivatives (ca. 20% in total). The exact positions of the chlorine atoms have been confirmed by X-ray diffraction of the corresponding single crystals. The acidity constants of all dicarboxylic acids in water were determined by capillary electrophoresis (3.17 ± 0.04 and 4.09 ± 0.05 for monochlorinated and ca. 2.71 ± 0.05 and 3.75 ± 0.05 for dichlorinated cubanes). All chlorinated derivatives as well as the parent diacid showed high thermal stability (decomposition above 250 °C) as documented by differential scanning calorimetry. The probable reaction pathways leading to individual isomers were proposed, and the energies of individual transition states and intermediates were obtained using density functional theory calculations (B3LYP-D3BJ/6-311+G(d,p)). The relative strain energies for all newly prepared derivatives as well as for hypothetical hexahalogenated (fluorinated, chlorinated, brominated, and iodinated) derivatives of cubane-1,4-dicarboxylic acids were predicted using wavefunction theory methods. The hexafluorinated derivative was identified as the most strained compound (57.5 kcal/mol), and the relative strain decreased as the size of halogen atoms increased (23.7 for hexachloro, 16.7 for hexabromo, and 4.0 kcal/mol for the hexaiodo derivative).
在此,我们报道了立方烷 - 1,4 - 二羧酸的自由基氯化反应,该反应优先生成一种单氯化立方烷二羧酸酯(约70%),同时伴有四种二氯化衍生物(总计约20%)。氯原子的确切位置已通过相应单晶的X射线衍射得以确认。通过毛细管电泳测定了所有二羧酸在水中的酸度常数(单氯化立方烷二羧酸为3.17 ± 0.04和4.09 ± 0.05,二氯化立方烷二羧酸约为2.71 ± 0.05和3.75 ± 0.05)。差示扫描量热法表明,所有氯化衍生物以及母体二酸均表现出高热稳定性(分解温度高于250°C)。提出了导致各个异构体的可能反应途径,并使用密度泛函理论计算(B3LYP - D3BJ/6 - 311 + G(d,p))获得了各个过渡态和中间体的能量。使用波函数理论方法预测了所有新制备衍生物以及立方烷 - 1,4 - 二羧酸的假设六卤代(氟代、氯代、溴代和碘代)衍生物的相对应变能。六氟代衍生物被确定为应变最大的化合物(57.5千卡/摩尔),并且随着卤原子尺寸的增加,相对应变减小(六氯代的为23.7,六溴代的为16.7,六碘代衍生物的为4.0千卡/摩尔)。