反应详情

温度

65 °C

48% hydrobromic acid (3 mL) was added to a solution of (5R)-5-[(E)-2-(4-tert-butylphenyl)-2-(5-chloro-6-methoxypyridin-2-yl)ethenyl]-1-methylpyrrolidin-2-one (152 mg) in 1,4-dioxane (6 mL), and the mixture was stirred at 65° C. for one hour. The reaction solution was poured into water, followed by extraction with ethyl acetate. The organic layer was dried over anhydrous magnesium sulfate and filtered. The filtrate was concentrated under reduced pressure. The resulting residue was purified by NH-silica gel column chromatography (chloroform:methanol=100:0→98:2) to give a colorless powder (151 mg). This was recrystallized from ethyl acetate-hexane to give the title compound as a colorless powder (99 mg).

1. extractionfollowed by extraction with ethyl acetate
2. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
3. filtrationfiltered
4. concentrationThe filtrate was concentrated under reduced pressure
5. customThe resulting residue was purified by NH-silica gel column chromatography (chloroform:methanol=100:0→98:2)