Reference 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.
2-Iodo-4-chlorobenzoic acid (10 g, 35.5 mmol) and HBTU (17.5 g, 46 mmol) were added to DMF (100 ml), followed by cyclopropylamine (2.6 g, 46 mmol) and DIPEA (17.5 ml, 92 mmol). The reaction was stirred overnight before being quenched with 2.0 NaOH (100 ml), extracted with DCM (3 x 200 ml), dried and solvent removed in vacuo to yield a dark yellow solid. This was passed through a pad of silica, eluting with DCM, the filtrate was concentrated in vacuo to yield a yellow solid. Ether (200 ml) Was added, the slurry was sonicated for 20 mins, iso-hexane (100 ml) was then added and the system was stirred for 10 mins, filtered and dried to give a colourless solid (9.3 g, 82%). NMR (CDCl3) 7.82 (s, IH), 7.34 (d, IH), 7.28 (d, IH), 5.99 (s, IH), 2.94 – 2.84 (m, IH), 0.91 – 0.84 (m, 2H), 0.71 – 0.66 (m, 2H); m/z 322.
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.