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
PROCEDURE
实验过程
To a solution of the 5-[(1R*,2S*)-2-(benzyloxy)cyclopentyl]-1-(tetrahydro-2H-pyran-2-yl)-1H-pyrazole (1.15 g, 3.52 mmol) prepared in Example 148a in dichloromethane (10 mL), trifluoroacetic acid (5.0 mL) was added at room temperature, and the reaction solution was stirred for 12 hours. The reaction solution was concentrated, and a saturated aqueous solution of sodium hydrogencarbonate (50 mL) was added to the residue, followed by extraction with ethyl acetate (50 mL). The thus obtained organic layer was washed with saturated saline (50 mL) and dried over anhydrous sodium sulfate. After vacuum concentration, the residue was purified with silica gel chromatography (hexane/ethyl acetate=1:1) to yield the title compound (840 mg, 98%) as a pale yellow oil.
WORKUP
后处理
- concentrationThe reaction solution was concentrated
- additiona saturated aqueous solution of sodium hydrogencarbonate (50 mL) was added to the residue
- extractionfollowed by extraction with ethyl acetate (50 mL)
- washThe thus obtained organic layer was washed with saturated saline (50 mL)
- dry with materialdried over anhydrous sodium sulfate
- concentrationAfter vacuum concentration
- customthe residue was purified with silica gel chromatography (hexane/ethyl acetate=1:1)