反应 #465969

反应方程式

sodium bicarbonate

oleum

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

HNO3

→

yellow solid

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

溶剂

ethyl acetate

H2SO4

反应条件

后处理

1. 1
   温度The mixture was cooled in an ice/water bath and to it
2. 2
   其他The cooled reaction mixture
3. 3
   萃取The product was extracted with ethyl acetate (2×150 mL)
4. 4
   干燥the combined extracts were dried (MgSO4)
5. 5
   浓缩concentrated

实验过程

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.

来源