Some common heterocyclic compound, 3149-28-8, name is 2-Methoxypyrazine, molecular formula is C5H6N2O, 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. Quality Control of 2-Methoxypyrazine
Preparation 37; 2-Methoxy-3- (3-methoxy-4-nitrophenyl) pyrazine (P37); 2,2, 6, 6-Tetramethylpiperidine (0.71 mL, 4.21 mmol) was added to a solution of n- butyllithium (1.6M, 2.6 mL, 4.16 mmol) in tetrahydrofuran (10 mL) at-30C. The mixture was allowed to warm up to 0C and stirred at that temperature for 15 minutes. The solution was then cooled to-70C, a solution of 2-methoxypyrazine (200 mg, 1.80 mmol) in tetrahydrofuran (5 mL) was added and then the mixture stirred at that temperature for 30 minutes. A solution of zinc chloride (500 mg, 3.67 mmol) in tetrahydrofuran (5 mL) was subsequently added at-70C and the mixture was then allowed to warm slowly to room temperature. A solution containing tetrakis (triphenylphosphine) palladium (0) (83 mg, 0.07 mmol) and 4-bromo-2-methoxy-1-nitrobenzene (459 mg, 1.98 mmol) in tetrahydrofuran (5 mL) was added to the organozinc derivative and the mixture heated at 65C for 2 hours. The reaction mixture was then hydrolyse with a solution containing ethylenediaminetetraacetic acid (1.1 g, 3.7 mmol) in water (10 mL) which had been made slightly basic with a saturated aqueous solution of potassium carbonate. The aqueous phase was extracted with dichloromethane (3×100 mL) and the combined extracts dried over magnesium sulfate and concentrated in vacuo. The product was purified by silica gel chromatography eluting with 0 to 80% ethyl acetate in hexane to yield the title compound as a solid ; MS (APCI+ve) : [M+H] + at m/z 262 (C12H11N304 requires [M+H] + at m/z 262).
These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 3149-28-8, its application will become more common.