Reaktion #3203

Reaktionsgleichung

chloral hydrate

sodium sulfate

3,5-dimethylaniline

HCl

hydroxylamine hydrochloride

→

title compound

Ausbeute 95.0%

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

Ausbeute 95.0%

Lösungsmittel

water

water

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigewhereupon an off-white precipitate formed
2. 2
   Temperaturheated
3. 3
   Temperaturat reflux for 10 min during which time the solids
4. 4
   workup.DISSOLUTIONdissolved
5. 5
   Sonstigea tan precipitate formed
6. 6
   TemperaturThe mixture was cooled
7. 7
   Filtrationfiltered
8. 8
   Sonstigedried

Vorschrift

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%).

Quelle