反应详情

To a solution of (E)-picolinaldehyde oxime (10.0 g, 82.0 mmol) in DMF (30 mL) at room temperature was slowly added over 30 minutes N-chlorosuccinamide (10.9 g, 82.0 mmol). An exotherm was noted during the addition. The reaction mixture was stirred overnight at room temperature, diluted with diethyl ether (300 mL), washed with water, dried over magnesium sulfate, and concentrated under reduced pressure. The residue was triturated with dichloromethane, and the resulting solid was collected by vacuum filtration and dried to give (Z)—N-hydroxypicolinimidoyl chloride (12.8 g, 51.1 mmol, 62% yield). 1H NMR (400 MHz, DMSO-d6) δ ppm 7.49 (ddd, 1H), 7.83-7.95 (m, 2H), 8.66 (ddd, J=4.73, 1.43, 1.32 Hz, 1H), and 12.64 (s, 1H).

1. additionAn exotherm was noted during the addition
2. washwashed with water
3. dry with materialdried over magnesium sulfate
4. concentrationconcentrated under reduced pressure
5. customThe residue was triturated with dichloromethane
6. filtrationthe resulting solid was collected by vacuum filtration
7. customdried