تفاعل #440186

معادلة التفاعل

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

acetic anhydride

→

2-hydroxymethyl-3-methyl-4-(2,2,3,3,3-pentafluoropropoxy)-pyridine

ظروف التفاعل

المعالجة

1. 1
   تركيزconcentrated
2. 2
   workup.DISSOLUTIONThe residue was dissolved in methanol (30 ml)
3. 3
   workup.ADDITION2 N aqueous sodium hydroxide (20 ml) was added
4. 4
   workup.STIRRINGthe mixture was stirred at room temperature for 2 hours
5. 5
   تركيزAfter concentration, water
6. 6
   workup.ADDITIONwas added to the residue
7. 7
   استخلاصthe mixture was extracted with ethyl acetate
8. 8
   تجفيفThe extract was dried over magnesium sulfate
9. 9
   workup.DISTILLATIONthe solvent was then distilled off
10. 10
    غسيلElution
11. 11
    أخرىwith chloroform-methanol (10:1) and recrystallization from isopropyl ether

الإجراء التجريبي

Concentrated sulfuric acid (2 drops) was added to a solution or 2,3-dimethyl-4-(2,2,3,3,3-pentafluoropropoxy)-pyridine-1-oxide (2.5 g) in acetic anhydride (8 ml) and the mixture was stirred at 110° C. for 2 hours and then concentrated. The residue was dissolved in methanol (30 ml), 2 N aqueous sodium hydroxide (20 ml) was added, and the mixture was stirred at room temperature for 2 hours. After concentration, water was added to the residue and the mixture was extracted with ethyl acetate. The extract was dried over magnesium sulfate, the solvent was then distilled off, and the residue was applied to a silica gel (50 g) column. Elution with chloroform-methanol (10:1) and recrystallization from isopropyl ether gave 1.6 g of 2-hydroxymethyl-3-methyl-4-(2,2,3,3,3-pentafluoropropoxy)-pyridine as a brown oil.

المصدر