Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 144690-33-5, name is Ethyl 4-(2-hydroxypropan-2-yl)-2-propyl-1-((2′-(1-trityl-1H-tetrazol-5-yl)-[1,1′-biphenyl]-4-yl)methyl)-1H-imidazole-5-carboxylate, A new synthetic method of this compound is introduced below., Quality Control of Ethyl 4-(2-hydroxypropan-2-yl)-2-propyl-1-((2′-(1-trityl-1H-tetrazol-5-yl)-[1,1′-biphenyl]-4-yl)methyl)-1H-imidazole-5-carboxylate
To BIT (130 g, 1 eq) was added acetone (650 mL, 5 vol) at 25C – 30C, and the mixture was dissolved. The reaction mixture was cooled to 0C – 5C, and a solution of potassium hydroxide (30.5 g, 3 eq) in desalting water (130 mL, 1 vol) was slowly added over 15 min. The reaction temperature was warmed to 40C – 45C, and the mixture was stirred at 40C – 45C for 5 hr. Using TLC (thin layer chromatography) (TLC eluent: 10% methanol/methylene chloride, detection method: UV), complete disappearance of BIT was confirmed. [0303] The precipitated solid was filtered, and the filtrate was concentrated under reduced pressure at 40C – 45C. To the obtained concentrated residue were added 25% brine (520 mL, 4 vol) and ethyl acetate (780 mL, 6 vol). After stirring for 10 min, the mixture was left standing for 5 min and partitioned. The aqueous layer was extracted with ethyl acetate (2×260 mL, 2×2 vol), and the extracts were combined with the organic layer. To the organic layer was added saturated aqueous sodium hydrogen carbonate (3×390 mL, 3×3 vol), and the mixture was stirred for 5 min, left standing and partitioned. To the organic layer was added saturated brine (650 mL, 5 vol), and the mixture was stirred for 5 min, left standing and partitioned. The organic layer was dried over sodium sulfate and filtered, and the filtrate was concentrated under reduced pressure at 40C – 45C to give crude product of BIC (115 g, 87%) as a white solid. The crude product was directly used for the next step.
The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.
Reference:
Patent; API Corporation; SEKI, Masahiko; EP2891650; (2015); A1;,
Imidazole – Wikipedia,
Imidazole | C3H4N2 – PubChem