反应详情

温度

50 °C

To a solution of 2-ethyl-4-{(E)-2-[3-(methoxymethoxy)-1-(2-methylphenyl)-1H-pyrazol-4-yl]ethenyl}-1,3-thiazole (0.81 g) in methanol (20 mL) was added concentrated hydrochloric acid (0.42 mL) at room temperature, and the mixture was stirred at 50° C. for 1 hr. The reaction mixture was evaporated under reduced pressure, saturated aqueous sodium hydrogen carbonate was added to the residue, and the mixture was extracted with ethyl acetate-tetrahydrofuran. The organic layer was washed with saturated brine, dried over anhydrous magnesium sulfate and concentrated. Recrystallization of the residue from tetrahydrofuran-hexane gave 4-[(E)-2-(2-ethyl-1,3-thiazol-4-yl)ethenyl]-1-(2-methylphenyl)-1H-pyrazol-3-ol (0.607 g, yield 86%) as colorless prism crystals. melting point: 174-176° C.

1. customThe reaction mixture was evaporated under reduced pressure, saturated aqueous sodium hydrogen carbonate
2. additionwas added to the residue
3. extractionthe mixture was extracted with ethyl acetate-tetrahydrofuran
4. washThe organic layer was washed with saturated brine
5. dry with materialdried over anhydrous magnesium sulfate
6. concentrationconcentrated
7. customRecrystallization of the residue from tetrahydrofuran-hexane