反应详情

温度

90 °C

Sodium hydroxide 3N (3.14 L, 9.43 mol) is added dropwise to a stirred suspension of hydroxylamine hydrochloride (675.55 g, 9.43 mol) in 0.5 L of water at 0° C. To this mixture is added dropwise a suspension of 2,6-dichlorobenzaldehyde (1500 g, 8.57 mol) in 7.5 L of ethanol and the reaction is heated at 90° C. overnight. The mixture is cooled to room temperature and then, concentrated to dryness. The solid is triturated in a mixture of H2O/EtOH, 10:1 (4.4 L), filtered and dried under high vacuum at 45° C. overnight. 1621.78 g of title compound (99% yield) is obtained as a white solid. MS (m/e): 190 (M+1)

1. additionTo this mixture is added dropwise
2. temperatureThe mixture is cooled to room temperature
3. concentrationconcentrated to dryness
4. customThe solid is triturated in a mixture of H2O/EtOH, 10:1 (4.4 L)
5. filtrationfiltered
6. customdried under high vacuum at 45° C. overnight