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 tert-butyl {[1-{[5-(1,3-dioxolan-2-yl)-2-furyl]sulfonyl}-4-fluoro-5-(2-fluoropyridin-3-yl)-1H-pyrrol-3-yl]methyl}methylcarbamate (1.23 g) in tetrahydrofuran (5 mL) was added 2 mol/L hydrochloric acid (5 mL) at room temperature and the mixture was stirred for 40 hr. A half of the reaction mixture was evaporated under reduced pressure, and extracted with ethyl acetate. The separated organic layer was washed with saturated aqueous sodium hydrogen carbonate solution and saturated brine, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (eluent: hexane-ethyl acetate=9:1→2:1) to give the title compound as a brown oil (yield 661 mg, 59%).
WORKUP
后处理
- customA half of the reaction mixture was evaporated under reduced pressure
- extractionextracted with ethyl acetate
- washThe separated organic layer was washed with saturated aqueous sodium hydrogen carbonate solution and saturated brine
- dry with materialdried over anhydrous magnesium sulfate
- concentrationconcentrated under reduced pressure
- customThe residue was purified by silica gel column chromatography (eluent: hexane-ethyl acetate=9:1→2:1)