Synthetic Route of 13421-13-1, 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. 13421-13-1 name is 4-Chloro-2-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.
1) Synthesis of 4-chloro-2-(4-methoxyphenylthio)benzoic acid (Reference Example compound 2-1) [0185] 4-chloro-2-iodobenzoic acid (20.0 g), 4-methoxybenzenethiol (8.71 ml), potassium hydroxide (15.4 g), copper powder (0.48 g) and water (240 ml) was stirred under reflux for 4 hr. The reaction mixture was poured into a mixed solution of ethyl acetate and 1M hydrochloric acid, and the organic layer was separated. The organic layer was washed with saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure and the residue was washed in diisopropyl ether and hexane (1:8) to give Reference Example compound 2-1 (18.8 g) as a white powder. 1H-NMR (CDCl3) delta (ppm) : 3.89 (3H, s), 6.69 (1H, d, J = 1.8 Hz), 7.01 (2H, d, J = 8.6 Hz), 7.09 (1H, dd, J = 2.0, 8.3 Hz, 7.50 (2H, d, J = 8.6 Hz), 8.04 (1H, d, J = 8.5 Hz).
At the same time, in my other blogs, there are other synthetic methods of this type of compound, 4-Chloro-2-iodobenzoic acid, and friends who are interested can also refer to it.
Reference:
Patent; Mitsubishi Tanabe Pharma Corporation; HAMADA, Maiko; TASHIRO, Kaoru; SAKASHITA, Hiroshi; KIUCHI, Masatoshi; TAKEDA, Shuzo; ADACHI, Kunitomo; EP2842937; (2015); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com