반응 #465939

반응 방정식

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

용매

hexamethylphosphoric acid triamide

반응 조건

후처리

1. 1
   여과Then, the insoluble matter was filtered off
2. 2
   농축the filtrate was concentrated
3. 3
   workup.ADDITIONWater was added to the residue
4. 4
   추출the mixture was extracted with ethyl acetate
5. 5
   건조The extract layer was dried over magnesium sulfate
6. 6
   workup.DISTILLATIONthe solvent was distilled off
7. 7
   세척Elution
8. 8
   기타with chloroform-methanol (10:1) and recrystallization from ethyl acetate-hexane

실험 절차

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.

출처