반응 #3203

반응 방정식

chloral hydrate

sodium sulfate

3,5-dimethylaniline

HCl

hydroxylamine hydrochloride

→

title compound

수율 95.0%

N-(3,5-dimethylphenyl)-2-(hydroxyimino)acetamide

수율 95.0%

용매

water

water

water

반응 조건

후처리

1. 1
   기타whereupon an off-white precipitate formed
2. 2
   온도heated
3. 3
   온도at reflux for 10 min during which time the solids
4. 4
   workup.DISSOLUTIONdissolved
5. 5
   기타a tan precipitate formed
6. 6
   온도The mixture was cooled
7. 7
   여과filtered
8. 8
   기타dried

실험 절차

To a solution of chloral hydrate (14.1 g, 85.24 mM) and sodium sulfate (88.2g, 7.53 eq.) in 270 mL of water was added a solution of 3,5-dimethylaniline in a solution of concentrated HCl (16 mL) and water (51 mL), whereupon an off-white precipitate formed. The mixture was stirred for 10 min prior to adding an aqueous solution of hydroxylamine hydrochloride (17.4 g, 250 mM) in water (50 mL) and then heated at reflux for 10 min during which time the solids dissolved and a tan precipitate formed. The mixture was cooled and filtered, and the collected solids were air dried to yield the title compound (15.0 g, 95%).

출처