تفاعل #3203

معادلة التفاعل

chloral hydrate

sodium sulfate

3,5-dimethylaniline

HCl

hydroxylamine hydrochloride

→

title compound

المردود 95.0%

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

المردود 95.0%

المذيبات

water

water

water

ظروف التفاعل

المعالجة

1. 1
   أخرىwhereupon an off-white precipitate formed
2. 2
   درجة الحرارةheated
3. 3
   درجة الحرارةat reflux for 10 min during which time the solids
4. 4
   workup.DISSOLUTIONdissolved
5. 5
   أخرىa tan precipitate formed
6. 6
   درجة الحرارةThe mixture was cooled
7. 7
   ترشيحfiltered
8. 8
   أخرىdried

الإجراء التجريبي

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%).

المصدر