双齿[C,N]和三齿[C,N,S]环金属钯配合物作为交叉偶联反应的预催化剂。

IF 2.5 4区 化学 Q2 CHEMISTRY, MULTIDISCIPLINARY
Basma al Janabi, Francisco Reigosa, Juan M. Ortigueira, José M. Vila
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引用次数: 0

摘要

卤化物取代的双齿[C,N]和三齿[C,N,S]席夫碱配体与醋酸钯或四氯palladate锂(视情况而定)分别通过C- h活化有机配体,双核(1a, 1b)和单核(1c, 1d, 1e)配体。μ-乙酸酯双核配合物与氯化钠水溶液在复分解过程中反应,得到μ-氯双核配合物(2a, 2b)。后者用三苯基膦或二(二苯基膦)甲烷(dppm)/六氟磷酸铵以配合物/膦1:1的比例处理,得到膦衍生物(3a, 3b, 4a, 4a)。c和e分别与三苯基膦/高氯酸银和dppm/高氯酸银反应,通过沉淀卤化银去除氯配体,得到化合物2c和2e。采用微量分析(CHN)、IR、1H和31P{1H} NMR对化合物进行了表征。用单晶x射线衍射研究了4 a、1 c和1 e三种配合物的晶体结构。此外,还测试了钯环作为预催化剂的性能,即Suzuki-Miyaura交叉偶联反应,并报道了效果较好的预催化剂。
本文章由计算机程序翻译,如有差异,请以英文原文为准。
Bidentate [C,N] and Tridentate [C,N,S] Palladium Cyclometallated Complexes as Pre-Catalysts in Cross-Coupling Reactions

Treatment of halide substituted bidentate [C,N] and tridentate [C,N,S] Schiff base ligands with palladium(II) acetate or with lithium tetrachloropalladate, as appropriate, afforded through C−H activation of the organic ligand, the dinuclear (1 a, 1 b) and mononuclear (1 c, 1 d, 1 e) palladacycles, respectively. Reaction of the μ-acetate dinuclear complexes with aqueous sodium chloride in a metathesis process, gave the μ-chloride dinuclear complexes (2 a, 2 b). Treatment of the latter with triphenylphosphine or with bis(diphenylphosphino)methane (dppm)/ammonium hexafluorophosphate in complex/ phosphine 1 : 2 ratio, gave the phosphine derivatives (3 a, 3 b, 4 a, 4 b). Reaction of 1 c and of 1 e with triphenylphosphine/silver perchlorate and dppm/silver perchlorate, respectively, gave compounds 2 c and 2 e with removal of the chloride ligand by precipitation of the silver halide. The compounds were characterized by microanalysis (CHN), IR and 1H and 31P{1H} NMR spectroscopy. The crystal structures of three complexes, 4 a, 1 c and 1 e were studied by single-crystal X-ray diffraction. Furthermore, the performance of the palladacycles were tested as pre-catalysts, namely Suzuki-Miyaura cross-coupling reaction and those furnishing the better results are also reported.

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来源期刊
ChemistryOpen
ChemistryOpen CHEMISTRY, MULTIDISCIPLINARY-
CiteScore
4.80
自引率
4.30%
发文量
143
审稿时长
1 months
期刊介绍: ChemistryOpen is a multidisciplinary, gold-road open-access, international forum for the publication of outstanding Reviews, Full Papers, and Communications from all areas of chemistry and related fields. It is co-owned by 16 continental European Chemical Societies, who have banded together in the alliance called ChemPubSoc Europe for the purpose of publishing high-quality journals in the field of chemistry and its border disciplines. As some of the governments of the countries represented in ChemPubSoc Europe have strongly recommended that the research conducted with their funding is freely accessible for all readers (Open Access), ChemPubSoc Europe was concerned that no journal for which the ethical standards were monitored by a chemical society was available for such papers. ChemistryOpen fills this gap.
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