Electric Literature of 113170-72-2, In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 113170-72-2 as follows.
Step A: 7-bromo-5-(trifluoromethyl)-1H-benzo[d]imidazol-2-amine (1099) To a 25 mL microwave tube was added a solution of 3-bromo-5-(trifluoromethyl)benzene-1,2-diamine (0.510 g, 2.0 mmol) in 6 mL of methanol, followed by addition of cyanic bromide (0.254 g, 2.40 mmol) and 4 mL of water. The mixture was stirred for 16 hr. TLC showed most SM was converted. The reaction mixture was heated at 80 C. for 1 hr and no SM was left. The solvent was removed via rotavapor and the residue was purified via column chromatography (ISCO RediSep gold column, 40 g) using 0-10% MeOH/DCM as mobile phase to afford the title compound. LC-MS (M+H)+: 280.10
According to the analysis of related databases, 113170-72-2, the application of this compound in the production field has become more and more popular.
Reference:
Patent; Merck Sharp & Dohme Corp.; Mandal, Mihir; Tang, Haifeng; Xiao, Li; Su, Jing; Li, Guoqing; Yang, Shu-Wei; Pan, Weidong; Tang, Haiqun; DeJesus, Reynalda; Hicks, Jacqueline; Lombardo, Matthew; Chu, Hong; Hagmann, William; Pasternak, Alex; Gu, Xin; Jiang, Jinlong; Dong, Shuzhi; Ding, Fa-Xiang; London, Clare; Biswas, Dipshikha; Young, Katherine; Hunter, David N.; Zhao, Zhiqiang; Yang, Dexi; (405 pag.)US2016/333021; (2016); A1;,
Bromide – Wikipedia,
bromide – Wiktionary