تفاعل #51599

معادلة التفاعل

2,2,3,3-tetrafluoropropan-1-ol

NaH

2,6-bis-(1-methyl-3-trifluoromethylpyrazol-5-yloxy)-4-methoxypyridine

→

title compound

المردود 99.2%

2-(1-Methyl-3-trifluoromethylpyrazol-5-yloxy)-4-methoxy-6-(2,2,3,3-tetrafluoropropyloxy)pyridine

المردود 99.2%

المذيبات

sulfolane

pentane ethyl acetate

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةis cooled to ambient temperature
2. 2
   ترشيحfiltered through a bed of silica gel
3. 3
   غسيلThe filtrate is washed 10 times with water
4. 4
   تجفيفThe organic layer is dried with anhydrous magnesium sulfate
5. 5
   ترشيحfiltered
6. 6
   أخرىevaporated in vacuo
7. 7
   أخرىPurification by flash chromatography (silica gel: pentane/ethyl acetate 9/1 v/v)

الإجراء التجريبي

To a mixture of 2,2,3,3-tetrafluoropropan-1-ol (0.29 g, 2.2 mmol) in dry sulfolane (2 ml) is added NaH (60% in oil, 0.09 g, 2.2 mmol) and 2,6-bis-(1-methyl-3-trifluoromethylpyrazol-5-yloxy)-4-methoxypyridine (0.8 g, 1.8 mmol). After stirring at 110° C. for 3.7 h the mixture is cooled to ambient temperature. The resulting mixture is diluted with pentane/ethyl acetate (by volume ration 1/1) and filtered through a bed of silica gel. The filtrate is washed 10 times with water. The organic layer is dried with anhydrous magnesium sulfate, filtered and evaporated in vacuo. Purification by flash chromatography (silica gel: pentane/ethyl acetate 9/1 v/v) yields the title compound (0.72 g, 57% yield) of m.p. 73-74° C.

المصدر