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 41270-66-0 as follows. Computed Properties of C16H11ClN2
In one embodiment of the preparation method of the sirepag intermediate of the present invention, the preparation method of the siriparg intermediate according to the present embodiment is: in a reaction bottle equipped with a reflux tube, a drying tube and a thermometer, adding 5- Chloro-2,3-diphenylpyrazine (30.0 g, 0.11 mol, 1.0 eq.), 4-(isopropylamino)-1-butanol (18.5 g, 0.14 mol, 1.25 eq.), 1, 4-Dioxane 150 mL, stir and dissolve, and then add Pd (dba)2(2.4g, 4.2mmol), P(o-tolyl)3(1.69 g, 8.3 mmol), sodium tert-butoxide (13.0 g, 0.135 mol), heated to 120 C., and incubated for 1.8 hours. The reaction was complete by TLC and the reaction was stopped.The mixture was cooled to room temperature and filtered. The filtrate was adjusted to pH 6.5-7.5 with 1N hydrochloric acid, extracted with ethyl acetate (150 mL x 2), washed with 150 mL of brine, and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure with the residue being ethanol: The mixture was recrystallized with 300 mL of n-hexane = 1:15 mixed solvent and dried in an oven to obtain 39.0 g of a white solid. The yield was 96%, and the liquid purity was 97.1%.
According to the analysis of related databases, 41270-66-0, the application of this compound in the production field has become more and more popular.
Reference:
Patent; Guangdong Saifeng Pharmaceutical Technology Co., Ltd.; Feng Wenzhou; Chen Rongmin; Ding Xiaoming; Zheng Yuchun; Bao Changxiao; Gong Zihua; (9 pag.)CN107652243; (2018); A;,
Pyrazine – Wikipedia,
Pyrazine | C4H4N2 – PubChem