반응 #51599

반응 방정식

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

NaH

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

→

title compound

수율 99.2%

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

수율 99.2%

용매

sulfolane

pentane ethyl acetate

반응 조건

후처리

1. 1
   온도is cooled to ambient temperature
2. 2
   여과filtered through a bed of silica gel
3. 3
   세척The filtrate is washed 10 times with water
4. 4
   건조The organic layer is dried with anhydrous magnesium sulfate
5. 5
   여과filtered
6. 6
   기타evaporated in vacuo
7. 7
   기타Purification by flash chromatography (silica gel: pentane/ethyl acetate 9/1 v/v)

실험 절차

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.

출처