反应详情

To a solution of the compound (30 mg) obtained in Example 6 in tetrahydrofuran (0.3 ml) was added, with stirring at room temperature, N,N′-carbonyldiimidazole (10 mg). After stirring at room temperature for 3 hr, 28% aqueous ammonia solution (10 μl) was added. After stirring at room temperature for 2.5 hr, 28% aqueous ammonia solution (10 μl) was added. After stirring at room temperature for 2.5 hr, 28% aqueous ammonia solution (10 μl) was added. After stirring overnight at room temperature, the reaction mixture was partitioned by adding ethyl acetate and saturated aqueous sodium hydrogen carbonate solution. The organic layer was washed successively with water and saturated brine, dried over anhydrous magnesium sulfate, filtrated, and concentrated under reduced pressure. The residue was purified by thin layer chromatography (10% methanol/chloroform) to give the title compound (20 mg).

1. stirringAfter stirring at room temperature for 3 hr
2. stirringAfter stirring at room temperature for 2.5 hr
3. stirringAfter stirring at room temperature for 2.5 hr
4. stirringAfter stirring overnight at room temperature
5. customthe reaction mixture was partitioned
6. additionby adding ethyl acetate and saturated aqueous sodium hydrogen carbonate solution
7. washThe organic layer was washed successively with water and saturated brine
8. dry with materialdried over anhydrous magnesium sulfate
9. filtrationfiltrated
10. concentrationconcentrated under reduced pressure
11. customThe residue was purified by thin layer chromatography (10% methanol/chloroform)