Hydrochloric Acid → Acetamide, 2-(hydroxyimino)-N-phenyl-

Temperatur

35 °C

Chloral hydrate (5.0 g) and Na2SO4 (35.0 g) were dissolved in water (70 mL) in a 300 mL beaker and warmed to 35° C. A warm solution of the appropriate commercial aniline derivative Ia-d (27.6 mmol) in water (20 mL) and aqueous solution of conc. HCl (3 mL) was added (a white precipitate of the amine sulfate was formed), followed by a warm solution of hydroxylamine hydrochloride (6.1 g) in water (27.5 mL). The mixture was stirred by hand and heated on a hot plate (a thick paste formed at 75-70° C.) at 80-90° C. for 2 h, then allowed to cool for 1 h, by which time the temperature had fallen to 50° C., and filtered. The pale cream product was washed by stirring with water (100 mL) and filtered. Drying overnight at 40° C. gave the corresponding isonitrosoacetanilide IIa-d.

1. customwas formed),
2. temperatureheated on a hot plate (a thick paste
3. customformed at 75-70° C.) at 80-90° C. for 2 h
4. temperatureto cool for 1 h, by which time the temperature
5. customhad fallen to 50° C.
6. filtrationfiltered
7. washThe pale cream product was washed
8. stirringby stirring with water (100 mL)
9. filtrationfiltered
10. customDrying overnight at 40° C.

ORD-Eintrag

ord-c203f26c124e4ef9a8ef8b3bf25aa4e3

Quelldatensatz

uspto-grants-2013_10

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08552053B2