447-60-9Relevant articles and documents
Preparation method of o-trifluoromethylbenzamide
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Paragraph 0067; 0072-0075, (2022/01/12)
The present invention discloses a method for preparing o-trifluoromethyl benzamide. The preparation method comprises the following steps: (1) in an organic solvent, the 2-nitrobenzotrifluoride and fluorinated salts are denitrified as shown below to obtain o-fluorobenzotrifluoride; (2) in an organic solvent, the o-fluortrifluorotoluene and cyanidylation reagent are defluoride cyanidation reaction as shown below to obtain o-trifluoromethylbenzonitrile; (3) in the presence of alkali, the o-trifluoromethylbenzonitrile, hydrogen peroxide hydrolysis reaction as shown below. The preparation method is simple to treat, the product purity is high, the impurities are small, and the yield is high.
Recyclable and Reusable Pd(OAc)2/XPhos–SO3Na/PEG-400/H2O System for Cyanation of Aryl Chlorides with Potassium Ferrocyanide
Cai, Mingzhong,Huang, Bin,Liu, Rong,Xu, Caifeng
, (2021/12/03)
Pd(OAc)2/XPhos–SO3Na in a mixture of poly(ethylene glycol) (PEG-400) and water is shown to be a highly efficient catalyst for the cyanation of aryl chlorides with potassium ferrocyanide. The reaction proceeded smoothly at 100 or 120?oC with K2CO3 or KOAc as base, delivering a variety of aromatic nitriles in good to excellent yields. The isolation of the crude products is facilely performed by extraction with cyclohexane and more importantly, both expensive Pd(OAc)2 and XPhos–SO3Na in PEG-400/H2O system could be easily recycled and reused at least six times without any apparent loss of catalytic efficiency. Graphical Abstract: Palladium-catalyzed cyanation of aryl chlorides with potassium ferrocyanide leading to aryl nitriles by using Pd(OAc)2/XPhos–SO3Na/PEG-400/H2O as a highly efficient and recyclable catalytic system is described.[Figure not available: see fulltext.]
Acceptorless dehydrogenation of amines to nitriles catalyzed by N-heterocyclic carbene-nitrogen-phosphine chelated bimetallic ruthenium (II) complex
Chen, Hua,Fu, Haiyan,Ji, Li,Li, Ruixiang,Nie, Xufeng,Zheng, Yanling
, p. 378 - 385 (2020/10/02)
We have developed a clean, atom-economical and environmentally friendly route for acceptorless dehydrogenation of amines to nitriles by combining a new dual N-heterocyclic carbene-nitrogen-phosphine ligand R(CNP)2 (R = o-xylyl) with a ruthenium precursor [RuCl2(η6-C6H6)]2. In this system, the electronic and steric factors of amines had a negligible influence on the reaction and a broad range of functional groups were well tolerated. All of the investigated amines could be converted to nitriles in good yield of up to 99% with excellent selectivity. The unprecedented catalytic performance of this system is attributed to the synergistic effect of two ruthenium centers chelated by R(CNP)2 and a plausible reaction mechanism is proposed according to the active species found via in situ NMR and HRMS.