Reaktion #51599

Reaktionsgleichung

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

NaH

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

→

title compound

Ausbeute 99.2%

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

Ausbeute 99.2%

Lösungsmittel

sulfolane

pentane ethyl acetate

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturis cooled to ambient temperature
2. 2
   Filtrationfiltered through a bed of silica gel
3. 3
   WaschenThe filtrate is washed 10 times with water
4. 4
   TrocknenThe organic layer is dried with anhydrous magnesium sulfate
5. 5
   Filtrationfiltered
6. 6
   Sonstigeevaporated in vacuo
7. 7
   SonstigePurification by flash chromatography (silica gel: pentane/ethyl acetate 9/1 v/v)

Vorschrift

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.

Quelle