Hydrochloric Acid → N-(3,5-dimethylphenyl)-2-(hydroxyimino)acetamide

温度

45 °C

Chloral hydrate (15.29 g, 92.42 mmol) was taken in water (335 mL). Sodium sulfate (78.14 g, 550.13 mmol) was added at room temperature. Then, a suspension of hydroxylamine hydrochloride (18.35 g, 264.06 mmol), 3.5-dimethylaniline (10.0 g, 82.52 mmol) and concentrated hydrochloric acid (36.5%, 10 mL) was added. The mixture was heated at 45° C. for 1.5 hours, then 75° C. for 1 hour. The reaction mixture was cooled to room temperature. The precipitated brown solid was filtered and washed with cold water (50 mL) and hexane (50 mL). The crude compound was dried under vacuum to give N-(3,5-dimethyl-phenyl)-2-hydroxyimino-acetamide as a brown solid. Yield: 13.7 g (86%). The crude compound was used in the next step without further purification.

1. additionwas added
2. temperatureThe reaction mixture was cooled to room temperature
3. filtrationThe precipitated brown solid was filtered
4. washwashed with cold water (50 mL) and hexane (50 mL)
5. dry with materialThe crude compound was dried under vacuum

ORDレコード

ord-163beeaeda8a4a8281861c700fc95e68

出典データセット

uspto-grants-2016_01

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US09238640B2