Reacción #52642

Ecuación de reacción

4-anisidine

hydrochloric acid

hydroxylamine hydrochloride

chloral hydrate

sodium sulfate

→

N—(2-hydroximinoacetyl)anisidine

Rendimiento 85.2%

Disolventes

water

water

water

Condiciones de reacción

Tratamiento posterior

1. 1
   Otrowas held at 60° C.
2. 2
   workup.ADDITIONThe first solution was then added to the second and the reaction
3. 3
   Temperaturawas refluxed for 2 minutes
4. 4
   Temperaturacooled in an ice bath
5. 5
   OtroThe tan precipitate which formed
6. 6
   Filtraciónwas collected by vacuum filtration
7. 7
   Lavadowashed with water
8. 8
   Otrodried under vacuum

Procedimiento

A solution of 11.4 g of hydroxylamine hydrochloride in water (50 ml) was added to a solution of chloral hydrate (9.6 g) and sodium sulfate (83 g) in water (200 ml) at 60° C. The mixture was held at 60° C. while, in a separate flask, a solution of 4-anisidine (6.4 g) and concentrated hydrochloric acid (4.3 ml) in water (80 ml) was warmed to 80° C. The first solution was then added to the second and the reaction was refluxed for 2 minutes, cooled slowly to room temperature and then cooled in an ice bath. The tan precipitate which formed was collected by vacuum filtration, washed with water and dried under vacuum to give 8.6 g (85% yield) of N—(2-hydroximinoacetyl)anisidine.

Fuente