Extracurricular laboratory: Synthetic route of C6H6N2O

At the same time, in my other blogs, there are other synthetic methods of this type of compound, Acetylpyrazine, and friends who are interested can also refer to it.

Related Products of 22047-25-2, 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. 22047-25-2 name is Acetylpyrazine, 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.

Step 1 Preparation of 4,4-difluoro-1-(2-pyrazinyl)-butane-1,3-dione Ethyl difluoroacetate (2.23 g, 18 mmol) was placed in a 100 mL round bottom flask and dissolved in ether (10 mL). To the stirred solution was added 25 weight % sodium methoxide (4.68 g, 22 mmol) followed by acetylpyrazine (2.00 g,16 mmol). After two hours stirring at room temperature, a precipitate formed and THF (10 mL) was added to the reaction. The reaction was stirred an additional 25.9 hours, then treated with 3N HCl (10 mL). The organic layer was collected, washed with brine (20 mL), dried over MgSO4, and concentrated in vacuo and recrystallized from methylene chloride/isooctane to give the diketone as a brown solid (2.23 g, mp 103-110 C., 68%) 1 H NMR (CDCl3) 300 MHz 14.00 (br s, 1H), 9.31 (d, J=1.4 Hz, 1H), 8.76 (d, J=2.4 Hz, 1H), 8.68 (dd, J= 1.4 Hz 2.4 Hz, 1H), 7.20 (s, 1H), 6.03 (t, J=54.0 Hz, 1H); 19 F NMR (CDCl3) 300 MHz: -127.16 (d); M+ 200.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, Acetylpyrazine, and friends who are interested can also refer to it.

Reference:
Patent; G.D. Searle & Co.; US5521207; (1996); A;,
Pyrazine – Wikipedia,
Pyrazine | C4H4N2 – PubChem