Abstract
双(二甲氧基苯基膦)二氯化钯(II)的合成及化学结构表征
Synthesis and Structure of Dichloridobis(dimethoxyphenylphosphine)palladium(II)
Received:October 25, 2017  
DOI:
中文关键词: 无机化学  双(二甲氧基苯基膦)二氯化钯(PdCl2[P(OMe)2Ph]2)  合成  化学结构  单晶
英文关键词: inorganic chemistry  PdCl2[P(OMe)2Ph]2  synthesis  chemical structure  single crystal
基金项目:国家科技支撑计划项目(2012BAE06B08)、云南省科技人才计划(2015HC022)。
Author NameAffiliationE-mail
JIN Xiaojuan 1. Kunming Institute of Precious Metals, State Key Laboratory of Advanced Technologies for ComprehensiveUtilization of Platinum Metals, Sino-Platinum Metals Co. Ltd., Kunming 650106, China jin_xjuan@163.com 
ZHANG Yangyang 1. Kunming Institute of Precious Metals, State Key Laboratory of Advanced Technologies for ComprehensiveUtilization of Platinum Metals, Sino-Platinum Metals Co. Ltd., Kunming 650106, China  
ZUO Chuan 1. Kunming Institute of Precious Metals, State Key Laboratory of Advanced Technologies for ComprehensiveUtilization of Platinum Metals, Sino-Platinum Metals Co. Ltd., Kunming 650106, China  
CHENG Yong 1. Kunming Institute of Precious Metals, State Key Laboratory of Advanced Technologies for ComprehensiveUtilization of Platinum Metals, Sino-Platinum Metals Co. Ltd., Kunming 650106, China  
HAN Xu 1. Kunming Institute of Precious Metals, State Key Laboratory of Advanced Technologies for ComprehensiveUtilization of Platinum Metals, Sino-Platinum Metals Co. Ltd., Kunming 650106, China  
GAO Anli 1. Kunming Institute of Precious Metals, State Key Laboratory of Advanced Technologies for ComprehensiveUtilization of Platinum Metals, Sino-Platinum Metals Co. Ltd., Kunming 650106, China  
YU Juan 1. Kunming Institute of Precious Metals, State Key Laboratory of Advanced Technologies for ComprehensiveUtilization of Platinum Metals, Sino-Platinum Metals Co. Ltd., Kunming 650106, China  
LIU Weiping 1. Kunming Institute of Precious Metals, State Key Laboratory of Advanced Technologies for ComprehensiveUtilization of Platinum Metals, Sino-Platinum Metals Co. Ltd., Kunming 650106, China  
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中文摘要:
      以氯亚钯酸钠、双甲氧基苯基膦酸盐为起始原料,通过配位取代反应合成了大配体C-C偶联催化剂双(二甲氧基苯基磷)二氯化钯(II) (PdCl2[P(OMe)2Ph]2)。优化的一步合成条件为:在氩气保护下,向双甲氧基苯基膦酸盐的四氢呋喃溶液中滴加0.5倍摩尔分数的氯亚钯酸钠水溶液,50℃反应得到配合物,产率为96.5%。采用核磁共振(1H NMR)及单晶X射线衍射(XRD)对产物化学结构进行测定和解析。1H NMR显示,2个苯环及4个甲氧基上的氢核信号的化学位移、峰面积与目标化合物对应一致;单晶XRD确定其晶体为单斜晶系空间群为C2/c,获得了相应的键长和键角参数。
英文摘要:
      Dichloridobis(dimethoxyphenylphosphine)palladium(II) (PdCl2[P(OMe)2Ph]2), a new type C-C coupling catalyst containing bulky organic phosphine, was synthesized via the ligand substitution reaction from sodium tetrachloropalladate(II) and dimethyl phenylphosphonite as the starting material. Under the Ar-protecting atmosphere a 0.5 mole fraction of sodium tetrachloropalladate(II) solution was added dropwise to the solution of dimethyl phenylphosphonite in tetrahydrofuran, and the yield was up to 96.5% based on the palladium content. The resulting compound was characterized by 1H NMR and single crystal X-ray diffraction analysis (XRD). 1H NMR revealed that the compound contains hydrogen signals due to two benzene rings and four methoxy groups. The results from XRD pattern demonstrated that the crystal form of the compound belongs to monoclinic with a space group of C2/c. Five atoms, P1, P2, Cl1, Cl2 and Pd, are almost in the same plane. The two benzene rings are staggered.
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