反应详情

A mixture of 2,6-bis(1-methyl-3-trifluoromethylpyrazol-5-yloxy)-4-methylpyridine (prepared according to WO 94/22833; 4.2 g, 10 mmol) and NaOH (1 g, 25 mmol) is heated in DMSO (50 ml) and water (5 ml) for 36 h at 100° C. After cooling, the reaction mixture is diluted with water and acidified with hydrochloric acid. The mixture is diluted with pentane/ethyl acetate (300 ml by volume ration 1/1) and the organic layer is washed 6 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 8/2 v/v and 7/3 v/v) yields the title compound (1.9 g, 70% yield) of m.p. 159° C.

1. temperatureAfter cooling
2. washthe organic layer is washed 6 times with water
3. dry with materialThe organic layer is dried with anhydrous magnesium sulfate
4. filtrationfiltered
5. customevaporated in vacuo
6. customPurification by flash chromatography (silica gel: pentane/ethyl acetate 8/2 v/v and 7/3 v/v)