Synthesis of Trispirocyclotriphosphazenes with Oxaphosphorine Rings and Their Crystal and Molecular Structures
作者:Yuji Tada、Atsushi Sunada、Riki Watanabe、Makoto Kanazawa、Keiichiro Utsumi
DOI:10.1021/acs.inorgchem.1c00054
日期:2021.4.5
were characterized by 1H, 13C1H}, and 31P1H} nuclear magnetic resonance spectroscopy and time-of-flight mass spectrometry and shown to consist of cis–trans isomers. Moreover, the crystal and molecular structures of the DOP-PZs were determined by X-ray diffraction; cis- and trans-DOP-PZs (C36H24N3O3P3, M = 639.49 g/mol) were refined to final R1 values of 0.0260 and 0.0463, respectively, with the SHELXL
通过氨与10-氯-9,10-二氢-9-氧杂-10-膦菲10氧化物从9衍生而来的磷酰胺的Appel反应成功地合成了具有氧杂磷环(DOP-PZs)的新型三螺环三磷腈(DOP-PZs)。 ,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide,通常缩写为DOPO。所得DOP-PZs的特征在于1 H,13 C 1 H}和31 P 1 H}核磁共振波谱和飞行时间质谱,并显示由顺-反异构体组成。此外,通过X射线衍射确定了DOP-PZ的晶体和分子结构。顺式和反式使用最小二乘最小化的SHELXL精制软件包,将-DOP-PZs(C 36 H 24 N 3 O 3 P 3,M = 639.49 g / mol)精制为最终R 1值0.0260和0.0463。的晶体顺-DOP-PZ是在空间群三角- [R 3 Ç和下面的晶胞常数:一个= 19.5984(5),C ^