Reference of 2034-22-2, 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. 2034-22-2 name is 2,4,5-Tribromoimidazole, 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.
A dried 500 mL round bottom flask was charged with 2,4,5-tribromoimidazole (5 1, 20.0 g, 65.6 mmol) and anhydrous DMF (100 mL), and the resulting solution was cooled to 0C. To this cold solution was added NaH (60% in mineral oil, 2.80 g, 70.0 mmol) portionwise with gas evolution under control and an internal temperature maintained below l0C. After addition, the cold bath was removed and the resulting mixture was stirred at ambient temperature for 30 minutes. The reaction mixture was cooled back to 0C, and SEMC1 (12.2 mL, 69.5 mmol) was added to the reaction via syringe pump over 30 minutes. The reaction was stirred at 0C for an additional 30 minutes and at room temperature for another 30 minutes. The mixture was partitioned between EtOAc (150 mL) and water (300 mL), the organic phase was washed with dilute aqueous NaCl (5percent w/w) twice, then brine (100 mL), dried (Na2S04), and concentrated. The crude material was re-crystallized from hot petroleum ether (30 mL) and the solids were harvested from the mother liquor at 0C. The product was washed with cold petroleum ether (30 mL) and dried under vacuum to afford 2,4,5-tribromo-l-((2-(trimethylsilyl)ethoxy)methyl)-lH-imidazole (5_2). 1H MR (400 MHz, CDCh) d 5.31 (s, 2H), 3.59 (t, J= 7.2 Hz, 2H), 0.92 (t, J= 7.2 Hz, 2H), -0.01 (s, 9H).
At the same time, in my other blogs, there are other synthetic methods of this type of compound, 2,4,5-Tribromoimidazole, and friends who are interested can also refer to it.
Reference:
Patent; MERCK SHARP & DOHME CORP.; LIU, Jian; CLAUSEN, Dane James; YU, Wensheng; KELLY, Joseph, M.; KIM, Hyunjin, M.; KOZLOWSKI, Joseph, A.; (202 pag.)WO2020/28150; (2020); A1;,
Imidazole – Wikipedia,
Imidazole | C3H4N2 – PubChem