反应 #1379890

反应方程式

sodium hydroxide

5-aminoquinoline

crotonic acid

water

→

cream solid

收率 51.0%

3-(quinolin-5-ylamino)-butyric Acid

收率 51.0%

溶剂

toluene

反应条件

后处理

1. 1
   温度at reflux for 48 h
2. 2
   温度to cool to ambient,
3. 3
   萃取the filtrate extracted with diethyl ether (3×100 ml)
4. 4
   其他The precipitate which formed
5. 5
   过滤was collected by filtration
6. 6
   洗涤washed first with water (200 ml)
7. 7
   干燥with acetone (200 ml) before being dried

实验过程

A mixture of 5-aminoquinoline (9.9 g, 0.069 mol) and crotonic acid (8.9 g, 0.103 mol) in toluene (35 ml) was stirred at reflux for 48 h. The reaction mixture was allowed to cool to ambient, added to water (500 ml) and the pH adjusted to 9 to 10 by the addition of 2N sodium hydroxide. The reaction mixture was screened and the filtrate extracted with diethyl ether (3×100 ml). The pH of the aqueous layer was first adjusted to pH2 with concentrated HCl and then to pH7 with calcium hydroxide. The precipitate which formed was collected by filtration, washed first with water (200 ml) and then with acetone (200 ml) before being dried to give 8.1 g of a cream solid.

来源