50438-47-6Relevant articles and documents
Preparation method of N-methyl-4-bromoaniline
-
Paragraph 0046; 0049; 0053; 0056; 0060; 0063, (2019/12/25)
The invention provides a preparation method of N-methyl-4-bromoaniline, belonging to the technical field of organic synthesis. The preparation method solves the technical problems that existing monomethylation reaction steps of aniline are tedious and the purity of prepared products is low. The method comprises the following steps: 1, adding dichloroethane and N-methylaniline into a first reactor,then dropwise adding acetic anhydride into the first reactor, and carrying out stirring; 2, dropwise adding a brominating agent into the formed reaction system, carrying out stirring, carrying out sampling analysis until the content of N-methyl acetanilide is less than 1%, adding sodium sulfite, carrying out stirring, and carrying out suction filtration; 3, adding the solid N-methyl-4-bromoacetanilide obtained through suction filtration in the step 2 into a second reactor, then adding hydrochloric acid with a mass concentration of 15%, carrying out heating reflux for 3 h, and carrying out sampling analysis until a reaction is completed; and 4, cooling, neutralizing and extracting the reaction system in the step 3, and recovering the solvent to obtain the colorless transparent liquid N-methyl-4-bromoaniline. The N-methyl-4-bromoaniline prepared by using the method is high in purity, and has a content of greater than 98%.
A para-C–H Functionalization of Aniline Derivatives via In situ Generated Bulky Hypervalent Iodinium Reagents
Tian, Chao,Yao, Xu,Ji, Weizhe,Wang, Qian,An, Guanghui,Li, Guangming
supporting information, p. 5972 - 5979 (2018/11/23)
A practical para-C-H functionalization of aniline derivatives has been developed using an in situ generated bulky hypervalent iodinium reagent. Para-iodo, bromo, chloro, nitro, trifluormethyl aniline derivatives can be obtained efficiently, in many cases in 10 min in a transition metal-free manner. Medicinal chemicals or intermediates can be purified without column chromatography or recrystallization, which significantly reduces the waste and simplifies the work-up process.
Thermolysis and radiofluorination of diaryliodonium salts derived from anilines
Linstad, Ethan J.,Vāvere, Amy L.,Hu, Bao,Kempinger, Jayson J.,Snyder, Scott E.,DiMagno, Stephen G.
supporting information, p. 2246 - 2252 (2017/03/17)
Aniline-derived diaryliodonium salts were synthesized and functionalized in good to excellent yields by judicious utilization of electron-withdrawing protecting groups. This simple approach opens another route to radiolabeling amino arenes in relatively complex molecules, such as flutemetamol.