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 4744-50-7 as follows. SDS of cas: 4744-50-7
EXAMPLE 1; Preparation of 3-(5-chloropyrid -2-yl) carbamoyl-pyrazine 2 carboxylic acid; In a clean, dry 500 ml R. B. flask charged acetic anhydride (162 gms) and pyrazine- 2,3, dicarboxylic acid (50 gms). The reaction mass was heated to 100-120 C. up to completion of reaction. After completion of reaction, the excess acetic anhydride was distilled under vacuum. Charged methylene dichloride (350 ml) to the above reaction mass followed by 2-amino-5- chloropyridine (40 gms) in a lot wise manner at room temperature in 30 min. The reaction mass was stirred at room temperature for 2 hrs; cooled the reaction mixture to 5-10 C. for 1 hr. The reaction mixture was filtered and washed with chilled methylene dichloride to obtain 3-(5-chloropyrid -2-yl) carbamoyl-pyrazine-2-carboxylic acid.Yield=82 gms.; EXAMPLE 2; Preparation of 6-(5-chloropyrid-2-yl) 5,7-dioxo-5,6-dihydropyrrolo [3,4-b]-pyrazine; In a clean 500 ml R. B.flask charged pyrazine-2,3-dicaroxylic acid (50 gms) and acetic anhydride (162 gms). The reaction mass was heated to 110-120 C. till the completion of reaction to get pyrazine-2,3-dicarboxylic acid anhydride. After completion of the reaction, excess acetic anhydride distilled out under vacuum and furthermore charged methylene dichloride (315 ml) and 2-amino-5-chloropyridine (40 gms) in a lot wise manner at room temperature in 30 min. Further, reaction mixture was stirred for 2 hours at room temperature. The reaction mass was cooled to 5 to 10 C. for one hour, filtered the product and washed with chilled methylene dichloride. The solid was charged with methylene dichloride (235 ml), triethylamine (40.9 ml) at temp. 0-5 C. followed by ethyl chloroformate (28.1 ml). The reaction mass was stirred at 0-5 C. for 1 hr, added water (200 ml) to the reaction mixture and stirred the mass at room temperature for 1 hr to obtain the solids. The title compound thus separated was isolated by filtration.Yield=65 gms.The HPLC purity of this above product was above 99%.
According to the analysis of related databases, 4744-50-7, the application of this compound in the production field has become more and more popular.
Reference:
Patent; Sawant, Shrikant Dattatraya; Naik, Anil Mahadev; Kavishwar, Girish Arvind; Kavishwar, Smita Girish; US2008/146800; (2008); A1;,
Pyrazine – Wikipedia,
Pyrazine | C4H4N2 – PubChem