反应详情

tert-Butyl ({4-fluoro-5-(2-fluoropyridin-3-yl)-1-[(6-methoxypyridin-3-yl)sulfonyl]-1H-pyrrol-3-yl}methyl)methylcarbamate (124 mg) was dissolved in ethyl acetate (1 mL) and ethanol (1 mL), and 4 mol/L hydrogen chloride-ethyl acetate solution (2 mL) was added. After stirring at room temperature for 2 hr, the reaction mixture was concentrated under reduced pressure. Saturated aqueous sodium hydrogen carbonate solution was added to the residue and the mixture was extracted with ethyl acetate. The extract was washed with saturated brine, dried over anhydrous sodium sulfate, and concentrated under reduced pressure to give the title compound as a free base (57.1 mg). A solution of the obtained free base (57.1 mg) in ethyl acetate (2 mL) was added dropwise to a solution of fumaric acid (24 mg) in ethanol (2 mL), and the mixture was concentrated under reduced pressure. The obtained crystal was recrystallized from a mixed solvent of ethanol-water=20:1 to give the title compound as colorless crystals (yield 24.4 mg, 33%).

1. concentrationthe reaction mixture was concentrated under reduced pressure
2. additionSaturated aqueous sodium hydrogen carbonate solution was added to the residue
3. extractionthe mixture was extracted with ethyl acetate
4. washThe extract was washed with saturated brine
5. dry with materialdried over anhydrous sodium sulfate
6. concentrationconcentrated under reduced pressure