تفاعل #440185

معادلة التفاعل

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

المذيبات

hexamethylphosphoric acid triamide

ظروف التفاعل

المعالجة

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

الإجراء التجريبي

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.

المصدر