反应 #465939

反应方程式

2,3-dimethyl-4-nitropyridine-1-oxide

methyl ethyl ketone

2,2,3,3,3-pentafluoropropanol

potassium carbonate

→

2,3-dimethyl-4-(2,2,3,3,3-pentafluoropropoxy)pyridine-1-oxide

溶剂

hexamethylphosphoric acid triamide

反应条件

后处理

1. 1
   过滤Then, the insoluble matter was filtered off
2. 2
   浓缩the filtrate was concentrated
3. 3
   workup.ADDITIONWater was added to the residue
4. 4
   萃取the mixture was extracted with ethyl acetate
5. 5
   干燥The extract layer was dried over magnesium sulfate
6. 6
   workup.DISTILLATIONthe solvent was distilled off
7. 7
   洗涤Elution
8. 8
   其他with chloroform-methanol (10:1) and recrystallization from ethyl acetate-hexane

实验过程

A mixture of 2,3-dimethyl-4-nitropyridine-1-oxide (2.0 g), methyl ethyl ketone (30 ml), 2,2,3,3,3-pentafluoropropanol (3.05 ml), anhydrous potassium carbonate (3.29 g) and hexamethylphosphoric acid triamide (2.07 g) was heated at 70-80° C. with stirring for 4.5 days. Then, the insoluble matter was filtered off and the filtrate was concentrated. Water was added to the residue and the mixture was extracted with ethyl acetate. The extract layer was dried over magnesium sulfate, then the solvent was distilled off, and the residue was applied to a silica gel column (50 g). Elution with chloroform-methanol (10:1) and recrystallization from ethyl acetate-hexane gave 2.4 g of 2,3-dimethyl-4-(2,2,3,3,3-pentafluoropropoxy)pyridine-1-oxide as colorless needles. Melting point 148-149° C.

来源