反应详情

Concentrated hydrochloric acid (0.50 mL) was added to an acetic acid (5.0 mL) solution of N-hydroxy-1-(1-methyl-1H-pyrazol-5-yl)-3-[4-(trifluoromethyl)phenyl]prop-2-yn-1-imine (303 mg) at a room temperature, and the obtained solution was then heated to reflux for 30 minutes. Thereafter, water was added to the reaction solution, and the obtained solution was then neutralized with potassium carbonate, followed by extraction with chloroform. The organic layer was washed with a saturated saline, and was then dried over anhydrous magnesium sulfate, followed by vacuum concentration. The residue was purified by column chromatography (silica gel cartridge, hexane:ethyl acetate=3:2), so as to obtain the title compound (229 mg) in the form of a colorless solid.

1. temperaturethe obtained solution was then heated
2. temperatureto reflux for 30 minutes
3. extractionfollowed by extraction with chloroform
4. washThe organic layer was washed with a saturated saline
5. dry with materialwas then dried over anhydrous magnesium sulfate
6. concentrationfollowed by vacuum concentration
7. customThe residue was purified by column chromatography (silica gel cartridge, hexane:ethyl acetate=3:2)