تفاعل #465956

معادلة التفاعل

2-ethylhexanol

sulfuric acid

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

→

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

المذيبات

water

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةAfter heating
2. 2
   أخرىthe reaction
3. 3
   درجة الحرارةto reflux overnight
4. 4
   درجة الحرارةthe reaction mixture was cooled
5. 5
   استخلاصextracted with ethyl acetate (75 mL)
6. 6
   غسيلThe organic phase was washed with sodium bicarbonate (75 mL)
7. 7
   تجفيفdried (Na2SO4)
8. 8
   تركيزconcentrated
9. 9
   أخرىThe resulting solid was recrystallized out of dichloromethane and hexane
10. 10
    ترشيحfiltered

الإجراء التجريبي

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).

المصدر