反应详情

温度

40 °C

Pyridine (7.75 g, 98.0 mmol) was added at 0° C. under N2 to a solution of 3-amino-pyrazine-2-carboxylic acid methyl ester 101 (1.5 g, 9.80 mmol) and 5-bromo-2-fluorobenzoylchloride (9.45 g, 49.0 mmol) in CH2Cl2. The reaction mixture was warmed at 40° C. for 4 h, then cooled down at room temperature. The reaction mixture was quenched with 20 mL of ethanol, evaporated, partitioned between CH2Cl2 and 1N NaHCO3, dried (Na2SO4) and evaporated. The crude material was triturated in EtOH, filtered, washed with EtOH and ether to give 2.6 g of 3-(5-bromo-2-fluorobenzoyl-amino)pyrazine-2-carboxylic acid methyl ester 102 as a white powder (LCMS analysis).

1. temperaturecooled down at room temperature
2. customThe reaction mixture was quenched with 20 mL of ethanol
3. customevaporated
4. custompartitioned between CH2Cl2 and 1N NaHCO3
5. dry with materialdried (Na2SO4)
6. customevaporated
7. customThe crude material was triturated in EtOH
8. filtrationfiltered
9. washwashed with EtOH and ether