反应详情

温度

85 °C

To a 250 mL round-bottomed flask was added 1-(3-fluoro-2-methylquinoxalin-5-yl)ethanone (126g) (14.5 g, 71 mmol), DMSO (100 mL), DIEA (27 mL, 156 mmol) and finally 1-methylcyclopropanamine hydrochloride (8.02 g, 92 mmol) (ChemBridge Corporation, San Diego, Calif.). The solution was heated at 85° C. for 7 h. After cooling to RT, the solution was poured into sat NaHCO3 (250 mL) and extracted with EtOAc (3×250 mL). The combined extracts were washed with H2O (3×250 mL) and brine and then dried (Na2SO4) and concentrated to afford 1-(2-methyl-3-((1-methylcyclopropyl)amino)-5-quinoxalinyl)ethanone (611a) as a purple solid, which was used directly in the subsequent step. m/z (ESI, +ve) 256.1 (M+H)+.

1. temperatureAfter cooling to RT
2. additionthe solution was poured
3. extractionextracted with EtOAc (3×250 mL)
4. washThe combined extracts were washed with H2O (3×250 mL) and brine
5. dry with materialdried (Na2SO4)
6. concentrationconcentrated