15617-18-2Relevant articles and documents
Preparation method of bis (cyanobenzene) palladium dichloride
-
Paragraph 0011-0017, (2021/04/03)
The invention discloses a preparation method of bis (cyanobenzene) palladium dichloride, which comprises the following steps: (1) dissolving palladium powder in aqua regia to prepare a palladium active group, cooling, and mixing with benzonitrile; (2) distilling to remove moisture, heating to react, and carrying out hot filtration; and (3) cooling the filtrate, adding the cooled filtrate into an organic solvent, separating out a solid, filtering, washing the obtained filter cake with the organic solvent, and carrying out vacuum drying. According to the method provided by the invention, palladium powder is used as a raw material to replace palladium chloride in the prior art, so that the reaction cost is reduced, and the prepared product is high in purity and high in yield.
Synthesis of a Bolm's 2,2′-Bipyridine Ligand Analogue and Its Applications
Bedná?ová, Eva,Dra?ínsky, Martin,Malatinec, ?tefan,Císa?ová, Ivana,Lamaty, Frédéric,Kotora, Martin
supporting information, p. 2869 - 2878 (2018/08/17)
A new method of synthesis of an analogue of Bolm's 2,2′-bipyridine ligand based on the catalytic [2+2+2] cyclotrimerization of 1-halodiynes with nitriles was developed. Crucial step of the whole synthesis turned out to be homodimerization of a substituted 2-bromopyridine to the corresponding bipyridine, that was studied and optimized. The newly prepared bipyridine (S,S)-2 was then tested as a chiral ligand in metal-catalyzed enantioselective reactions. Out of the studied reactions the most promising results were obtained in epoxide ring opening (82% yield, 98% ee) and Mukaiyama aldol reaction (>96% yield, 99/1 dr, 92% ee). In the case of Mukaiyama-aldol reaction as well as in the Michael addition, novel ligand 2 proved its robustness compared to Bolm's ligand as it was less sensitive to the purity of used reagents. (Figure presented.).
Preparation and application of coconut shell activated carbon immobilized palladium complexes
Zhang, Yulian,Xiang, Shuanglong,Wang, Guoqing,Jiang, Hong,Xiong, Chunrong
, p. 1055 - 1063 (2014/04/03)
Coconut shell activated carbon (CSAC) granules were used as carriers to immobilize palladium complexes. Boehm titration showed that the hydroxyl content of the carbon surface reached 0.376 mmol g-1 after 20% HNO 3 treatment. Ethylenediamine, benzyl malononitrile and propyl malononitrile were successfully grafted onto the oxidized CSAC. The bidentate nitrogen ligands complexed Pd2+ samples were characterized by FT-IR, XPS, ICP and N2 adsorption-desorption. In oxidative carbonylation of phenol, three bidentate ligand grafted catalysts were evaluated in a high pressure reaction vessel. The results showed that the ethylenediamine grafted catalyst had a phenol conversion of 12.06% and a diphenyl carbonate (DPC) selectivity of 91.03%. In comparison, the benzyl malononitrile grafted catalyst displayed a phenol conversion of 12.00% and a DPC selectivity of 90.65%. The propyl malononitrile grafted catalyst displayed a phenol conversion of 6.22% and a DPC selectivity of 81.02%. Additionally, the ethylenediamine and the benzyl malononitrile grafted catalysts were also investigated in a continuous packed-bed reactor. The results showed that the phenol conversion and the DPC selectivity were comparative to those obtained in a high pressure reaction vessel. This journal is the Partner Organisations 2014.
