反应详情

To a suspension of 5 mg of lithium aluminum hydride in 1 mL of tetrahydrofuran was added 13 mg of aluminum chloride (III), followed by 9 mg of 6-fluoro-3-[(E)-2-(3-fluorophenyl)-vinyl]-1H-indazole-5-carbonitrile obtained by Example 100, and stirred at room temperature overnight. After adding saturated aqueous ammonium chloride, the reaction solution was added with 15 mL of ethylacetate. The organic layer was washed successively with saturated aqueous sodium hydrogen carbonate (twice) and saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated, and the crude product was purified and separated by silica gel column chromatography (methanol:chloroform=1:9), to afford 3 mg of the title compound as a yellow oil.

1. washThe organic layer was washed successively with saturated aqueous sodium hydrogen carbonate (twice) and saturated brine
2. dry with materialdried over anhydrous magnesium sulfate
3. customThe solvent was evaporated
4. customthe crude product was purified
5. customseparated by silica gel column chromatography (methanol:chloroform=1:9)