反应详情

To 2-hydroxyquinolin-4-oyl chloride (V-A, 0.90 g) in dichloromethane (20 ml) are added dimethylamine hydrochloride (0.52 g), followed by diisopropylethylamine (1.12 ml). After stirring for 5 hr aqueous sodium bicarbonate is added and the mixture is extracted several times with dichloromethane. The organic layers are dried over sodium sulfate and concentrated. The crude product was chromatographed (silica gel; methanol/dichloromethane (2/98 to 4/96)), to give dimethylamino 2-hydroxyquinoline-4-carboxamide (VI, 0.73 g), mp 219-220°.

1. additionis added
2. extractionthe mixture is extracted several times with dichloromethane
3. dry with materialThe organic layers are dried over sodium sulfate
4. concentrationconcentrated
5. customThe crude product was chromatographed (silica gel; methanol/dichloromethane (2/98 to 4/96))