Reaktion #52642

Reaktionsgleichung

4-anisidine

hydrochloric acid

hydroxylamine hydrochloride

chloral hydrate

sodium sulfate

→

N—(2-hydroximinoacetyl)anisidine

Ausbeute 85.2%

Lösungsmittel

water

water

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigewas held at 60° C.
2. 2
   workup.ADDITIONThe first solution was then added to the second and the reaction
3. 3
   Temperaturwas refluxed for 2 minutes
4. 4
   Temperaturcooled in an ice bath
5. 5
   SonstigeThe tan precipitate which formed
6. 6
   Filtrationwas collected by vacuum filtration
7. 7
   Waschenwashed with water
8. 8
   Sonstigedried under vacuum

Vorschrift

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.

Quelle