7343-34-2, In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 7343-34-2 as follows.
In a 25 mL round-bottomed flask under N2 at 0 ¡ãC, sodium hydride (60percent in mineral oil, 0.059 g, 1.48 mmol) was added to a solution of 3,5-dimethyl-lH-l,2,4-triazole (0.112 g, 1.15 mmol) in DMF (5 mL) and the mixture was stirred for 30 min. To this mixture was then added 5-bromo-4′-(bromomethyl)-[l, r-biphenyl]-2-carbonitrile (1-002, 0.407 g, 1.16 mmol) and the mixture was stirred at RT for 3.5 h. The resulting mixture was then poured into H20 and the product was extracted with EtOAc (x3). The combined organic extract was washed with 0 (x3) and brine, dried over anhydrous sodium sulfate and concentrated to dryness. The residue was purified on ISCO using a 40 g column (0-5percent MeOH-DCM) to afford the title compound (0.248 mg, 0.675 mmol, 59percent yield) as a colorless gum. LC (Method B): 1.795 min. MS (APCI): calcd for Ci8H16BrN4 [M + H]+ m/z 367.1, found 367.0. H NMR (400 MHz, CDC13) delta ppm 7.66 (dd, J = 0.78, 1.57 Hz, 1H), 7.61 – 7.63 (m, 2H), 7.51 – 7.56 (m, 2H), 7.28 – 7.31 (m, 2H), 5.29 (s, 2H), 2.42 (s, 3H), 2.38 (s, 3H).
At the same time, in my other blogs, there are other synthetic methods of this type of compound, 7343-34-2, and friends who are interested can also refer to it.
Reference:
Patent; UNIVERSITE DE MONTREAL; BRISTOL-MYERS SQUIBB COMPANY; PRIESTLEY, Eldon, Scott; REZNIK, Samuel, Kaye; RUEDIGER, Edward, H.; GILLARD, James, R.; HALPERN, Oz, Scott; JIANG, Wen; RICHTER, Jeremy; RUEL, Rejean; TRIPATHY, Sasmita; YANG, Wu; ZHANG, Xiaojun; (642 pag.)WO2018/5591; (2018); A1;,
1,2,3-Triazole – Wikipedia,
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