HRID34026
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
CONDITIONS
反应条件
- 温度
- 80 °C
PROCEDURE
实验过程
3.60 g of 7-fluoro-3-[(E)-2-(pyridin-3-yl)-vinyl]-1-trityl-1H-indazole-5-carbonitrile was dissolved in 500 mL of ethanol, added with 154 g of potassium hydroxide, and stirred at 80° C. overnight. After cooling to room temperature, the solution was adjusted to pH 3 by 5N hydrochloric acid, and extracted with ethyl acetate. The organic layer was washed with water and saturated brine, dried over magnesium sulfate, and the solvent was evaporated. The obtained crude product was purified by silica gel column chromatography, and the resultant dark brown solid was washed with 10 mL of diethyl ether, to afford 3.58 g of the title compound as dark brown crystals.
WORKUP
后处理
- temperatureAfter cooling to room temperature
- extractionextracted with ethyl acetate
- washThe organic layer was washed with water and saturated brine
- dry with materialdried over magnesium sulfate
- customthe solvent was evaporated
- customThe obtained crude product
- customwas purified by silica gel column chromatography
- washthe resultant dark brown solid was washed with 10 mL of diethyl ether