تفاعل #709339

معادلة التفاعل

chloroform

3,5-dimethyl-4-nitropyridine-1-oxide

potassium t-butoxide

2,2,3,3,3-pentafluoropropanol

→

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

المردود 80.6%

ظروف التفاعل

المعالجة

1. 1
   أخرىThe resulting reaction product
2. 2
   ترشيحwas subjected to Celite filtration
3. 3
   غسيلwas eluted with ethyl acetate-hexane (1:1)
4. 4
   أخرىwith 20% methanol-ethyl acetate and then recrystallized from ether-hexane

الإجراء التجريبي

To a solution of 3,5-dimethyl-4-nitropyridine-1-oxide (2.0 g) in 2,2,3,3,3-pentafluoropropanol (10 g), potassium t-butoxide (2 g) was added gradually at 0° C. over a period of 15 minutes, after which the solution was stirred at 60° C. for 18 hours. The resulting reaction product, after adding chloroform, was subjected to Celite filtration, after which the filtrate was applied on a silica gel (80 g) column, was eluted with ethyl acetate-hexane (1:1) and then with 20% methanol-ethyl acetate and then recrystallized from ether-hexane to give 2.6 g of 3.5-dimethyl-4-(2,2,3,3,3-pentafluoropropoxy)pyridine-1-oxide as crystals (melting point: 89°~91° C.).

المصدر