反应 #465956

反应方程式

2-ethylhexanol

sulfuric acid

4-amino-3,6-dichloro-pyridine-2-carboxylic acid

→

2-ethylhexyl 4-amino-3,6-dichloropyridine-2-carboxylate

溶剂

water

反应条件

后处理

1. 1
   温度After heating
2. 2
   其他the reaction
3. 3
   温度to reflux overnight
4. 4
   温度the reaction mixture was cooled
5. 5
   萃取extracted with ethyl acetate (75 mL)
6. 6
   洗涤The organic phase was washed with sodium bicarbonate (75 mL)
7. 7
   干燥dried (Na2SO4)
8. 8
   浓缩concentrated
9. 9
   其他The resulting solid was recrystallized out of dichloromethane and hexane
10. 10
    过滤filtered

实验过程

To a solution of 2-ethylhexanol (10 mL) and sulfuric acid (1 mL) was added 4-amino-3,6-dichloro-pyridine-2-carboxylic acid (0.0097 mol, 2.0 g). After heating the reaction to reflux overnight, the reaction mixture was cooled, poured into water (75 mL), and extracted with ethyl acetate (75 mL). The organic phase was washed with sodium bicarbonate (75 mL), dried (Na2SO4), and concentrated. The resulting solid was recrystallized out of dichloromethane and hexane and filtered to give 2-ethylhexyl 4-amino-3,6-dichloropyridine-2-carboxylate (0.0074 mol, 2.36 g) as a crystalline solid (mp 55° C.). 1H NMR (CDCl3): δ 0.9 (7 H, m), 1.3 (7 H, m), 1.7 (1 H, m), 4.3 (2 H, d), 5.1 (2 H, bs), 6.7 (1 H, s).

来源