Electric Literature of 34270-90-1, 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. 34270-90-1 name is 1-Iodo-2-(2-iodoethoxy)ethane, 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.
To a solution of Intermediate 34 (2.60 g, 10.9 mmol) in DML (20 mL) was added sodium hydride (1.04 g, 21.7 mmol) at 0C. The reaction mixture was stirred at r.t. for 30 minutes, then l-iodo-2-(2-iodoethoxy)ethane (5.31 g, 16.3 mmol) was added. The reaction mixture was heated at 80C for 16 h, then poured into ice and extracted with EtOAc (3 x 100 mL). The combined organic layers were separated, washed with water (100 mL) and brine (100 mL), then dried over anhydrous Na2S04and concentrated in vacuo. The crude residue was purified by flash chromatography on silica (0-20% EtOAc in hexanes) to afford the title compound (2.00 g, 60%) as a yellow oil. 6n (400 MHz, DMSO-de) 1.06 (t, J7.09 Hz, 3H), 1.95-2.02 (m, 2H), 2.17-2.22 (m, 2H), 3.64-3.71 (m, 2H), 3.72-3.80 (m, 2H), 3.85 (s, 3H), 4.05 (q, J6.85 Hz, 2H), 7.66 (d, J8.80 Hz, 1H),7.75 (s, 1H), 7.83-7.88 (m, 1H).
At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1-Iodo-2-(2-iodoethoxy)ethane, and friends who are interested can also refer to it.
Reference:
Patent; UCB BIOPHARMA SRL; BRACE, Gareth Neil; BROOKINGS, Daniel Christopher; FOULKES, Gregory; LECOMTE, Fabien Claude; (0 pag.)WO2020/11731; (2020); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com