反应详情

To the compound (2.64 g) obtained in Step 2 in 1,4-dioxane (13 ml) was added, with stirring at room temperature, 4N hydrogen chloride/1,4-dioxane (13 ml). After stirring at room temperature for 3 hr, the reaction mixture was concentrated under reduced pressure. Toluene was added to the residue, and the mixture was concentrated again under reduced pressure. The residue 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 column chromatography (5%-10% methanol/chloroform) to give the title compound (1.59 g).

1. stirringAfter stirring at room temperature for 3 hr
2. concentrationthe reaction mixture was concentrated under reduced pressure
3. additionToluene was added to the residue
4. concentrationthe mixture was concentrated again under reduced pressure
5. customThe residue 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 column chromatography (5%-10% methanol/chloroform)