反应详情

温度

110 °C

To a suspension of 89 mg of 6-fluoro-3-[(E)-2-(3-fluorophenyl)-vinyl]-1H-indazole-5-carbonitrile obtained by Example 100 in 0.4 mL of acetic acid and 0.4 mL of water was added 1.2 mL of concentrated sulfuric acid, and stirred at 110° C. for 50 minutes. After allowing to cool, ice was added, and extracted with a mixed solvent of 20 mL of ethyl acetate and 10 mL of tetrahydrofuran. The organic layer was washed successively with water, saturated aqueous sodium hydrogen carbonate and saturated brine, and dried over anhydrous magnesium sulfate. After making the organic layer pass through an alumina pad (2.5 diameter ×2 cm), the solvent was evaporated, to afford 76 mg of the title compound as pale yellow crystals.

1. temperatureto cool
2. additionice was added
3. extractionextracted with a mixed solvent of 20 mL of ethyl acetate and 10 mL of tetrahydrofuran
4. washThe organic layer was washed successively with water, saturated aqueous sodium hydrogen carbonate and saturated brine
5. dry with materialdried over anhydrous magnesium sulfate
6. customthe solvent was evaporated