Synthetic Route of 23426-63-3, 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 23426-63-3 as follows.
To a 20-L reactor containing dimethyl formamide (4.5 L) was charged 5-methyl-4-nitro- lH-pyrazole la (1.5 kg, 1.0 equiv). The solution was cooled to 0 C and charged with finely ground K2CO3 (2.45 kg, 1.5 equiv) in three portions over ~l h. Methyl 2-bromo-2- methylpropanoate (3.2 kg, 1.5 equiv) was added dropwise to the mixture and then was allowed to warm to ~25 C. The reaction mixture was maintained for 16 h and then quenched with water (15 L) and product was extracted with ethyl acetate. The combined organic layer was washed with water, and then with a brine. The organic layer was dried over anhydrous Na2S04, filtered, and concentrated under reduced pressure to give a light yellow solid. The crude product was purified by crystallization with petroleum ether (15 L), filtered, and dried to give methyl 2- m ethyl -2-(3 -methyl -4-nitro- l//-pyrazol- l -yl)propanoate 3a (2.25 kg, >99% purity by HPLC, 84 % yield) as an off-white solid. NMR (400 MHz, CDCb) 8.28 (s, 1H), 3.74 (s, 3H), 2.53 (s, 3H), 1.85 (s, 6H).
According to the analysis of related databases, 23426-63-3, the application of this compound in the production field has become more and more popular.
Reference:
Patent; DENALI THERAPEUTICS INC.; REMARCHUK, Travis; SUDHAKAR, Anantha; (28 pag.)WO2019/126383; (2019); A1;,
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