Related Products of 4949-13-7, A common heterocyclic compound, 4949-13-7, name is 2-Fluoropyrazine, molecular formula is C4H3FN2, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.
10264] To a 2.5 M solution of n-butyllithium (40 mE, 0.1 mol) in anhydrous THF (250 mE) cooled to -78 C. under N2 protection was added TMP (2,2,6,6-tetramethylpiperidine, 15 g, 0.106 mol) dropwise over a period of 20 minutes. The mixture was warmed to 0 C. by replacing the dry ice/acetone bath with an ice bath and stirred for 1.5 h. The mixture was cooled back to -78C. and a solution of 9a (3 g, 0.03 mol) and tributyltin chloride (10 g, 0.03 mol) in SOmE of dry THF was added over 10 mm. The mixture was stirred at -78 C. for 6 h, then warmed to -40 C. by replacing the dry ice/acetone bath with an dry ice/acetonitrile bath. A solution of 35% HC1, ethanol and THF (1:4:5) was added. The mixture was warmed to room temperature and washed with saturated NaHCO3 solution (100 mE) and extracted with EtOAc (3×100 mE). The combined organic layers were dried over anhydrous Na2504 and concentrated under reduced pressure. The residue was purified by column chromatography (silica, EtOAc:petroleum ether=1:15) to provide 9b (3.4 g, 29% yield) as light yellow oil. ?H-NMR (CDC13, 300 MHz): oe=8.41 (d, 1H), 8.17 (d, 1H), 1.8-0.53 (m, 27H).
The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.
Reference:
Patent; Helsinn Healthcare SA; Giuliano, Claudio; Garcia Rubio, Silvina; Daina, Antoine; Guainazzi, Angelo; Pietra, Claudio; US2015/252021; (2015); A1;,
Pyrazine – Wikipedia,
Pyrazine | C4H4N2 – PubChem