Electric Literature of 16982-21-1, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 16982-21-1 name is Ethyl 2-amino-2-thioxoacetate, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.
Ethyl thiooxamate (1.0 Kg, 7.52 mol) was added portion-wise to a solution of 2- bromopyruvic acid (1.38 Kg, 8.27 mol) in THF (4 L) over 20 min while the reaction was cooled with water bath. The reaction mixture was stirred for 12 h at room temperature. The reaction mixture was filtered to remove solid. The filtrate was concentrated to dryness to afford crude compound 70-1 (1.8 kg). The crude 70-1 was triturated with EtOAc/hexane/H20 (1 :3 :2, 6 L), filtered, and the solid was further triturated with EtO Ac/hexane (1 :8, 3 L), filtered, and the solid was dissolved in DCM (6 L), dried over anhydrous Na2S04, concentrated to afford compound 70-1 (617 g, 41% yield based on ethyl thiooxamate) as light yellow solid. 1H NMR (400 MHz, CDCI3): d 8.79 (s, 1H), 4.38-4.46 (q, J= 7.2 Hz, 2H), 1.3-1.38 (t, J= 7.2 Hz, 3H).
At the same time, in my other blogs, there are other synthetic methods of this type of compound, Ethyl 2-amino-2-thioxoacetate, and friends who are interested can also refer to it.
Reference:
Patent; ARIAGEN, INC.; COLABUONO, Peter; JOHNSON, Graham; MANNING, David Douglas; WOLF, Mark Allan; (312 pag.)WO2019/99977; (2019); A2;,
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