作者:S. N. Ignat’eva、A. S. Balueva、A. A. Karasik、D. V. Kulikov、A. V. Kozlov、Sh. K. Latypov、P. Lönnecke、E. Hey-Hawkins、O. G. Sinyashin
DOI:10.1007/s11172-007-0284-9
日期:2007.9
Condensation of bis(hydroxymethyl)mesityl-and bis(hydroxymethyl)phenylphosphines with N,N′-disubstituted bis(4-aminophenyl)methanes and bis(4-amino-3-carboxyphenyl)methane occurred as covalent self-assembly spontaneously giving a mixture of trans-and cis-diastereomers of 1,5,19,23-tetra-R′-3,21-di-R-1,5,19,23-tetraaza-3,21-diphospha[5.1.5.1]paracyclophanes as the major products. The trans-isomer (R is mesityl; R′ is methyl) was isolated in the individual state and structurally characterized by X-ray diffraction analysis. Sulfurization of macrocyclic diphosphines (R = Ph; R′ is 3-pyridylmethyl or 4-pyridylmethyl) gave the corresponding diphosphine disulfides, the trans-stereoisomer being isolated in the individual state.
双(羟甲基)间甲苯胺和双(羟甲基)苯基膦与 N、N′-二取代双(4-氨基苯基)甲烷和双(4-氨基-3-羧基苯基)甲烷以共价自组装的方式自发发生缩合,产生了反式和顺式-非对映异构体的混合物,其主要产物为 1,5,19,23-四-R′-3,21-二-R-1,5,19,23-四氮杂-3,21-二磷杂[5.1.5.1]paracyclophanes 为主要产物。反式异构体(R 为甲苯甲基;R′ 为甲基)以单个状态分离出来,并通过 X 射线衍射分析确定了其结构特征。大环二磷酸(R = Ph;R′为 3-吡啶基甲基或 4-吡啶基甲基)的硫化反应得到了相应的二磷酸二硫化物,反式异构体以单个状态分离出来。