반응 #52642

반응 방정식

4-anisidine

hydrochloric acid

hydroxylamine hydrochloride

chloral hydrate

sodium sulfate

→

N—(2-hydroximinoacetyl)anisidine

수율 85.2%

용매

water

water

water

반응 조건

후처리

1. 1
   기타was held at 60° C.
2. 2
   workup.ADDITIONThe first solution was then added to the second and the reaction
3. 3
   온도was refluxed for 2 minutes
4. 4
   온도cooled in an ice bath
5. 5
   기타The tan precipitate which formed
6. 6
   여과was collected by vacuum filtration
7. 7
   세척washed with water
8. 8
   기타dried under vacuum

실험 절차

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.

출처