反应详情

To a solution of O,N-dimethyl-hydroxylamine hydrochloride salt (29 g, 0.30 mol, 1.1 eq) and DIEA (182 mL, 1.08 mol, 4.0 eq) in DCM (300 mL) was added the mixture of 3-chloro-quinoxaline-6-carbonyl chloride and 2-chloro-quinoxaline-6-carbonyl chloride (52 g, 0.27 mol, 1.0 eq) at 0° C. The mixture was stirred at rt overnight, then concentrated. The residue was washed with water (300 mL×2) and extracted with EA (300 mL×2). The combined organic layers were dried over anhydrous Na2SO4, filtered and concentrated. The resulting solid was triturated with EA/PE=1/1 (300 mL) to afford 3-chloro-N-methoxy-N-methylquinoxaline-6-carboxamide (16.5 g, 24.3%).

1. concentrationconcentrated
2. washThe residue was washed with water (300 mL×2)
3. extractionextracted with EA (300 mL×2)
4. dry with materialThe combined organic layers were dried over anhydrous Na2SO4
5. filtrationfiltered
6. concentrationconcentrated
7. customThe resulting solid was triturated with EA/PE=1/1 (300 mL)