反应详情

温度

150 °C

A mixture of 0.24 g of 3-amino-5-(trifluoromethyl)pyridine-2-thiol, 0.27 g of 5-ethylthio-1-methyl-3-trifluoromethyl-1H-pyrazole-4-carboaldehyde, 0.19 g of sodium sulfite, 0.33 g of copper(II) chloride (anhydrous) and 2 ml of N,N-dimethylacetamide was stirred at 150° C. for 8 hours. Ethyl acetate and a saturated aqueous sodium bicarbonate solution were poured into the cooled reaction mixture, and the mixture was filtered. The aqueous layer of the filtrate was extracted with ethyl acetate and then combined with the organic layer of the filtrate, and the mixture was washed with water and dried over anhydrous magnesium sulfate. The mixture was concentrated under reduced pressure, then the resulting residue was applied to a silica gel column chromatography to obtain 0.21 g of 2-(5-ethylthio-1-methyl-3-trifluoromethyl-1H-pyrazol-4-yl)-6-trifluoromethylthiazolo[5,4-b]pyridine (Compound of Present Invention (27)).

1. filtrationthe mixture was filtered
2. extractionThe aqueous layer of the filtrate was extracted with ethyl acetate
3. washthe mixture was washed with water
4. dry with materialdried over anhydrous magnesium sulfate
5. concentrationThe mixture was concentrated under reduced pressure