反应详情

To a stirred solution of 6-hydroxynicotinic acid (5.0 g, 1.0 eq), EDCI (8.3 g, 1.2 eq) and HOBt (5.8 g, 1.2 eq) in 150 mL CH2Cl2 were added N-methoxymethanamine hydrochloride (4.2 g, 1.2 eq) and Et3N (14.5 g, 4.0 eq) at rt, the mixture was stirred at rt overnight, water was added, and the mixture was extracted with CH2Cl2. The extract was dried, concentrated, and purified by column chromatography to give the desired product (3.5 g, 53% yield). 1H NMR (400 MHz, DMSO-d6) δ 11.82 (brs, 1H), 7.87 (d, J=2.8 Hz, 1H), 7.72 (dd, J=9.6 Hz, 2.8 Hz, 1H), 6.32 (d, J=9.6 Hz, 1H), 3.59 (s, 3H), 3.20 (s, 3H).

1. extractionthe mixture was extracted with CH2Cl2
2. customThe extract was dried
3. concentrationconcentrated
4. custompurified by column chromatography