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 4949-13-7 as follows. Recommanded Product: 2-Fluoropyrazine
A solution of 2-fluoropyrazine (0.247 mL, 3.06 mmol), 2-amino-1-(piperidin-1-yl)ethanone hydrochloride (710 mg, 3.98 mmol) and DIPEA (1.603 mL, 9.18 mmol) in acetonitrile (5 mL) was heated to 100 C for 16 h. The reaction mixture was concentrated and then dissolved in ethyl acetate (15 mL) and water (20 mL). The organic Layer was washed and separated. The aqueous layer was then washed with ethyl acetate (5 x 15 mL). The organic layers were combined, dried through a hydrophobic frit and concentrated in vacuo. The crude material was purified using silica chromatography with a gradient of 0-80 % (3:1 ethyl acetate:ethanol + 1 % triethylamine)/cyclohexane. The relevant fractions were combined and concentrated in vacuo to yield 1-(piperidin-1-yl)-2-(pyrazin-2-ylamino)ethanone (415 mg, 1.88 mmol, 61 % yield) as an orange solid. LCMS (High pH, ES+): tR = 0.67 min, [M+H]+ 221.16. 1H NMR (400 MHz, CDCl3) delta 1.55-1.64 (m, 4H), 1.65-1.73 (m, 2H), 3.39-3.44 (m, 2H), 3.60-3.66 (m, 2H), 4.13 (d, J = 3.79 Hz, 2H), 5.88 (br. s., 1H), 7.79 (d, J = 3.03 Hz, 1H), 7.95-7.98 (m, 1H), 8.02 (d, J = 1.26 Hz, 1H) 13C NMR (101 MHz, CDCl3) delta 24.4, 25.5, 26.2, 42.5, 43.3, 45.4, 132.6, 134.0, 141.4, 153.8, 166.6 HRMS: (C11H16N4O) [M+H]+ requires 221.1397, found [M+H]+ 221.1391 numax (neat): 3328, 2941, 2857, 1639, 1586, 1531, 1436, 1251, 1230, 1000, 820, 615 cm-1.
According to the analysis of related databases, 4949-13-7, the application of this compound in the production field has become more and more popular.
Reference:
Article; Law, Robert P.; Ukuser, Sabri; Tape, Daniel T.; Talbot, Eric P. A.; Synthesis; vol. 49; 16; (2017); p. 3775 – 3793;,
Pyrazine – Wikipedia,
Pyrazine | C4H4N2 – PubChem