反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 80 °C
PROCEDURE
实验过程
Acetic acid (2.6 ml) and water (0.7 ml) were added to a solution of 5-(4-benzyl-1-piperazinyl)-1-tetrahydro-2H-pyran-2-yl-1H-indazole (100 mg, 0.266 mmol) in tetrahydrofuran (1.3 ml) at room temperature and stirred 80° C. for 7 hours. Then, the reaction solution was concentrated and the resulting residue was diluted with ethyl acetate and washed with a saturated aqueous sodium hydrogencarbonate solution and then a saturated aqueous sodium chloride solution. The organic layer was dried over anhydrous sodium sulfate and distilled under reduced pressure to remove the solvent, and the resulting residue was purified by a thin-layer chromatography (eluent: chloroform/methanol=95/5) to obtain 5-(4-benzyl-1-piperazinyl)-1H-indazole (37 mg, 47%).
WORKUP
后处理
- concentrationThen, the reaction solution was concentrated
- additionthe resulting residue was diluted with ethyl acetate
- washwashed with a saturated aqueous sodium hydrogencarbonate solution
- dry with materialThe organic layer was dried over anhydrous sodium sulfate
- distillationdistilled under reduced pressure
- customto remove the solvent
- customthe resulting residue was purified by a thin-layer chromatography (eluent: chloroform/methanol=95/5)