反应 #52642

反应方程式

4-anisidine

hydrochloric acid

hydroxylamine hydrochloride

chloral hydrate

sodium sulfate

→

N—(2-hydroximinoacetyl)anisidine

收率 85.2%

溶剂

water

water

water

反应条件

后处理

1. 1
   其他was held at 60° C.
2. 2
   workup.ADDITIONThe first solution was then added to the second and the reaction
3. 3
   温度was refluxed for 2 minutes
4. 4
   温度cooled in an ice bath
5. 5
   其他The tan precipitate which formed
6. 6
   过滤was collected by vacuum filtration
7. 7
   洗涤washed with water
8. 8
   其他dried under vacuum

实验过程

A solution of 11.4 g of hydroxylamine hydrochloride in water (50 ml) was added to a solution of chloral hydrate (9.6 g) and sodium sulfate (83 g) in water (200 ml) at 60° C. The mixture was held at 60° C. while, in a separate flask, a solution of 4-anisidine (6.4 g) and concentrated hydrochloric acid (4.3 ml) in water (80 ml) was warmed to 80° C. The first solution was then added to the second and the reaction was refluxed for 2 minutes, cooled slowly to room temperature and then cooled in an ice bath. The tan precipitate which formed was collected by vacuum filtration, washed with water and dried under vacuum to give 8.6 g (85% yield) of N—(2-hydroximinoacetyl)anisidine.

来源