反応 #3203

反応方程式

chloral hydrate

sodium sulfate

3,5-dimethylaniline

HCl

hydroxylamine hydrochloride

→

title compound

収率 95.0%

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

収率 95.0%

溶媒

water

water

water

反応条件

後処理

1. 1
   その他whereupon an off-white precipitate formed
2. 2
   温度heated
3. 3
   温度at reflux for 10 min during which time the solids
4. 4
   workup.DISSOLUTIONdissolved
5. 5
   その他a tan precipitate formed
6. 6
   温度The mixture was cooled
7. 7
   ろ過filtered
8. 8
   その他dried

実験手順

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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