反应 #3203

反应方程式

chloral hydrate

sodium sulfate

3,5-dimethylaniline

HCl

hydroxylamine hydrochloride

→

title compound

收率 95.0%

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

收率 95.0%

溶剂

water

water

water

反应条件

后处理

1. 1
   其他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
   其他a tan precipitate formed
6. 6
   温度The mixture was cooled
7. 7
   过滤filtered
8. 8
   其他dried

实验过程

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%).

来源