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

温度

110 °C

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.

1. temperatureis cooled to ambient temperature
2. filtrationfiltered through a bed of silica gel
3. washThe filtrate is washed 10 times with water
4. dry with materialThe organic layer is dried with anhydrous magnesium sulfate
5. filtrationfiltered
6. customevaporated in vacuo
7. customPurification by flash chromatography (silica gel: pentane/ethyl acetate 9/1 v/v)

ORDレコード

ord-facc9139d28f472d8d74f9b9d1df1032

出典データセット

uspto-grants-2005_02

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US06852673B2