反应详情

温度

0 °C

To a 0° C. cooled and stirred, solution of 2,6-difluorobenzoyl chloride (5.7 g, 36.2 mmol, 0.9 eq) in DCM (200 mL) was added drop wise a solution of 2-amino-5-bromopyrazine (7.0 g, 40.2 mmol, 1.0 eq) in DCM (50 mL) followed b pyridine (3.1 g, 36.2 mmol, 0.9 eq). The resulting mixture was stirred at room temperature for 15 h. The reaction was diluted with DCM (100 mL), and washed with 10% hydrochloric acid (100 mL), dried (Na2SO4) and filtered. The filtrate was concentrated under vacuum and the crude product was purified by flash column chromatography (silica gel, 10% ethyl acetate in hexane) to afford 6.0 g of the title product as a yellow solid. 1HNMR (400 MHz, CDCl3) δ 9.47 (s, 1H), 8.62 (s, 1H, D2O exchangeable), 8.24 (s, 1H), 7.53-7.45 (m, 1H), 7.03 (t, J=8.0 Hz, 2H); ESI-MS (m/z) 314, 316 [(MH)+ Br79,81].

1. stirringThe resulting mixture was stirred at room temperature for 15 h
2. washwashed with 10% hydrochloric acid (100 mL)
3. dry with materialdried (Na2SO4)
4. filtrationfiltered
5. concentrationThe filtrate was concentrated under vacuum
6. customthe crude product was purified by flash column chromatography (silica gel, 10% ethyl acetate in hexane)