反应详情

25 mL H2O was added to chloral hydrate (1.49 g, 9 mmol) and anhydrous sodium sulfate (7.62 g, 54 mmol), and the mixture was rapidly stirred until clear. Hydroxylamine hydrochloride (6.84 g, 42 mmol) was added into dilute hydrochloric acid (9 mL H2O: 1 mL concentrated HCl), and then, aniline (1.23 g, 8 mmol) was added. The mixture was stirred to form a suspension. The suspension was added into an aqueous solution of chloral hydrate. After stirring for 5 min, the mixture was transferred to an oil bath at 45° C. and heated for 2 h. The reaction was finished by TLC detection, and the reaction system was stirred and cooled in an ice bath, filtered and dried, to obtain a solid oximino acetanilide.

1. stirringThe mixture was stirred
2. customto form a suspension
3. stirringAfter stirring for 5 min
4. customthe mixture was transferred to an oil bath at 45° C.
5. temperatureheated for 2 h
6. stirringthe reaction system was stirred
7. temperaturecooled in an ice bath
8. filtrationfiltered
9. customdried