Реакция #3203

Уравнение реакции

chloral hydrate

sodium sulfate

3,5-dimethylaniline

HCl

hydroxylamine hydrochloride

→

title compound

Выход 95.0%

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

Выход 95.0%

Растворители

water

water

water

Условия реакции

Обработка

1. 1
   Другоеwhereupon an off-white precipitate formed
2. 2
   Температураheated
3. 3
   Температураat reflux for 10 min during which time the solids
4. 4
   workup.DISSOLUTIONdissolved
5. 5
   Другоеa tan precipitate formed
6. 6
   ТемператураThe mixture was cooled
7. 7
   Фильтрацияfiltered
8. 8
   Другоеdried

Методика

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%).

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