Synthesis
5-(4'-Methylbiphenyl-2-yl)-1-trityl-1H-tetrazole is prepared by the reaction of trityl chloride and 2-(tetrazol-5-yl)-4'-methyl-1,1'-biphenyl. The specific synthesis steps are as follows:
Dissolve compound 2 (200 g) with stirring at 40°C 700mL of acetone, Aqueous sodium hydroxide solution (40.67 g sodium hydroxide dissolved in 160 mL water) is added, Continue stirring for 1h, A solution of triphenylchloromethane in acetone (270.8 g of triphenylmethyl chloride dissolved in 800 mL of acetone) was initially added dropwise. The solid was added dropwise and gradually evolved into a white turbid liquid. The reaction was monitored by TLC until it was completely filtered off and washed with water to give a solid as intermediate 3. The solid was blow dried at 50°C to give white intermediate 3 (385 g), yield: 95.2%, HPLC: 99.44%.
References
[1] Patent: WO2013/78237, 2013, A1. Location in patent: Page/Page column 111; 112
[2] Patent: CN107935957, 2018, A. Location in patent: Paragraph 0020; 0040-0042
[3] Synthetic Communications, 2008, vol. 38, # 20, p. 3577 - 3581
[4] Journal of Chemical Sciences, 2011, vol. 123, # 4, p. 393 - 401
[5] Archiv der Pharmazie, 2016, vol. 349, # 12, p. 934 - 943
