反应详情

Sodium hypochlorite (14% available chlorine, 35 mL, 82.21 mmol) solution was added to a stirred solution of 2-hydroxynicotinic acid (7 g, 50.3 mmol) in 10% aqueous NaOH solution. The solution was stirred for 48 h at room temperature. An aqueous solution of sodium sulfite (3.150 g, 25 mmol) was added and further stirred for 30 min at room temperature. The solution was diluted by cold water and pH was adjusted to 2 by cold dilute HCl. The solids formed were filtered, washed by cold water and dried to yield 6.8 g (78%) of 5-chloro-2-hydroxy-nicotinic acid (70) as white solids. MP: 276° C.; 1H-NMR (DMSO-d6): δ 8.23 (d, J=2.8 Hz, 1H), 8.29 (d, J=2.8 Hz, 1H); EIMS: 174 (M+1).

1. stirringfurther stirred for 30 min at room temperature
2. customThe solids formed
3. filtrationwere filtered
4. washwashed by cold water
5. customdried