反应 #452183

反应方程式

ammonia

Ammonium persulphate

4-cyanobutyric acid

4-dimethylaminomethylpyridine

sulphuric acid

→

2-(3-cyanopropyl)-4-dimethylaminomethylpyridine

收率 36.9%

溶剂

water

water

water

反应条件

后处理

1. 1
   workup.STIRRINGThe reaction mixture was stirred at 80° for 1.5 hours
2. 2
   温度cooled
3. 3
   workup.ADDITIONpoured
4. 4
   萃取The solution was extracted with chloroform (900 ml)
5. 5
   洗涤the chloroform extracts were washed with dilute sodium hydroxide
6. 6
   干燥dried over magnesium sulphate
7. 7
   浓缩concentrated in vacuo

实验过程

Ammonium persulphate (54.8 g) in water (150 ml) and 4-cyanobutyric acid (68 g) in water (300 ml) were added separately and simultaneously over 30 minutes to a mixture of 4-dimethylaminomethylpyridine (16.32 g), silver nitrate (4 g), water (200 ml) and concentrated sulphuric acid (25 ml) stirred at 80°. The reaction mixture was stirred at 80° for 1.5 hours, cooled, poured onto crushed ice (400 g) and aqueous ammonia (28% w/w, 200 ml). The solution was extracted with chloroform (900 ml) and the chloroform extracts were washed with dilute sodium hydroxide, dried over magnesium sulphate, and concentrated in vacuo to give 2-(3-cyanopropyl)-4-dimethylaminomethylpyridine (9 g) as a clear oil b.p. 110°-112°/0.1 mm Hg.

来源