تفاعل #465969

معادلة التفاعل

sodium bicarbonate

oleum

Methyl 3,6-dichloropyridine-2-carboxylate N-oxide

HNO3

→

yellow solid

4-Nitro-3,6-dichloropyridine-2-carboxylic Acid

المذيبات

ethyl acetate

H2SO4

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةThe mixture was cooled in an ice/water bath and to it
2. 2
   أخرىThe cooled reaction mixture
3. 3
   استخلاصThe product was extracted with ethyl acetate (2×150 mL)
4. 4
   تجفيفthe combined extracts were dried (MgSO4)
5. 5
   تركيزconcentrated

الإجراء التجريبي

Methyl 3,6-dichloropyridine-2-carboxylate N-oxide (5.0 g, 22.52 mmol) was dissolved in a minimum amount of H2SO4. The mixture was cooled in an ice/water bath and to it was slowly added 30% oleum (9.6 mL) and fuming HNO3 (9.6 mL), gradually heated to 65° C. and stirred for 48 hr. The cooled reaction mixture was diluted with ethyl acetate (200 mL) and to it was carefully added saturated sodium bicarbonate. The product was extracted with ethyl acetate (2×150 mL) and the combined extracts were dried (MgSO4) and concentrated to give 0.10 g of a yellow solid; mp 192-193° C.

المصدر