반응 #52596

반응 방정식

Chloral hydrate

hydroxylamine hydrochloride

4-anisidine

hydrochloric acid

→

N-(2-hydroximino-acetyl)anisidine

수율 85.2%

용매

water

sodium sulfate

water

water

반응 조건

후처리

1. 1
   기타was held at 60° C
2. 2
   workup.ADDITIONThe first solution was added to the second and the mixture
3. 3
   온도refluxed for 2 minutes after which it
4. 4
   온도was cooled slowly to room temperature
5. 5
   온도cooled in an ice bath
6. 6
   여과The tan precipitate was collected by vacuum filtration
7. 7
   세척washed with water
8. 8
   기타dried under vacuum

실험 절차

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

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