547710-68-9Relevant academic research and scientific papers
A chromatography-free and aqueous waste-free process for thioamide preparation with Lawesson's reagent
Wu, Ke,Ling, Yichen,Ding, An,Jin, Liqun,Sun, Nan,Hu, Baoxiang,Shen, Zhenlu,Hu, Xinquan
, p. 805 - 812 (2021/05/03)
After completing the thio-substitution with Lawesson's reagent, ethanol was found to be effective in the decomposition of the inherent stoichiometric six-membered-ring byproduct from the Lawesson's reagent to a highly polarized diethyl thiophosphonate. The treatment significantly simplified the following chromatography purification of the desired thioamide in a small scale preparation. As scaling up the preparation of two pincer-type thioamides, we have successfully developed a convenient process with ethylene glycol to replace ethanol during the workup, including a traditional phase separation, extraction, and recrystallization. The newly developed chromatography-free procedure did not generate P-containing aqueous waste, and only organic effluents were discharged. It is believed that the optimized procedure offers the great opportunity of applying the Lawesson's reagent for various thio-substitution reactions on a large scale.
Synthesis, characterization and application of nickel(II) complexes modified with N,N′,N″-pincer ligands
Czerny, Frank,D?hlert, Peter,Weidauer, Maik,Irran, Elisabeth,Enthaler, Stephan
supporting information, p. 118 - 123 (2015/02/02)
Different N,N″-substituted pyridine-2,6-dicarboxamides 1a-d have been synthesized and treated with nickel(II) trifluoromethanesulfonate in the presence of an excess of tetraethylammonium hydroxide to form after double-deprotonation the nickel hydroxido complexes 4a-c. These square planar complexes have been characterized by various techniques, which indicate a tridentate N,N′,N″-coordination mode of the ligands. The other coordination site on the nickel center is occupied by a hydroxido ligand. The reactivity of the complexes was studied in dehalogenation reactions and allows access to square planar nickel chlorido complexes 5a-c. Moreover, by NMR studies it was found that nickel hydroxido complexes as well as chlorido complexes can be converted with diphenylsilane or lithium borohydride to nickel hydrido complexes, which can be seen as a possible catalytic intermediate in reduction chemistry. Based on that, the potential of complexes 4 and 5 were evaluated in the hydrosilylation of ketones to produce alcohols after work-up.
Synthesis of bis(N-arylcarboximidoylchloride)pyridine cobalt(ii) complexes and their catalytic behavior for 1,3-butadiene polymerization
Liu, Heng,Jia, Xiangyu,Wang, Feng,Dai, Quanquan,Wang, Baolin,Bi, Jifu,Zhang, Chunyu,Zhao, Liping,Bai, Chenxi,Hu, Yanming,Zhang, Xuequan
, p. 13723 - 13732 (2013/09/23)
A new family of bis(N-arylcarboximidoylchloride)pyridine cobalt(ii) complexes with the general formula [2,6-(ArNCCl)2C5H 3N]CoCl2 (Ar = 2,4,6-Me3C6H 2, 4a; 2,6-iPrsub
