Synthetic Route of 1258298-01-9, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 1258298-01-9 name is 2,6-Dichloro-4-iodobenzoic acid, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.
General procedure: A mixture of 2-chloropyridine-3,4-diamine(2.80 g, 19.4mmol), 2,6-dichlorobenzoic acid(3.71 g, 19.4mmol)andpolyphosphoricacid (50 g) was heated at 190 Cfor 3 h with stirring. The mixture was cooled to room temperature and poured into ice/water. The resulting mixture was neutralized by addition of aq. saturated Na2CO3solution. The crude product was collected by filtration, washed with water, and dried to afford a brown solid(5.4 g, 97% yield).1H NMR(DMSO-d6, 500 MHz):delta13.08 (s, 1H), 11.21 (s, 1H), 7.67-7.58 (m, 3H),7.15 (m, 1H), 6.49 (d,J= 7.0 Hz, 1H).LCMS(ESI) m/z: 280.0 [M+H+].
At the same time, in my other blogs, there are other synthetic methods of this type of compound, 2,6-Dichloro-4-iodobenzoic acid, and friends who are interested can also refer to it.
Reference:
Article; Liang, Jun; Van Abbema, Anne; Balazs, Mercedesz; Barrett, Kathy; Berezhkovsky, Leo; Blair, Wade S.; Chang, Christine; Delarosa, Donnie; DeVoss, Jason; Driscoll, Jim; Eigenbrot, Charles; Goodacre, Simon; Ghilardi, Nico; MacLeod, Calum; Johnson, Adam; Bir Kohli, Pawan; Lai, Yingjie; Lin, Zhonghua; Mantik, Priscilla; Menghrajani, Kapil; Nguyen, Hieu; Peng, Ivan; Sambrone, Amy; Shia, Steven; Smith, Jan; Sohn, Sue; Tsui, Vickie; Ultsch, Mark; Williams, Karen; Wu, Lawren C.; Yang, Wenqian; Zhang, Birong; Magnuson, Steven; Bioorganic and Medicinal Chemistry Letters; vol. 27; 18; (2017); p. 4370 – 4376;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com