反应详情

To a solution of the compound (1.59 g) obtained in Step 3 in chloroform (16 ml) was added, with stirring at room temperature, triethylamine (840 μl), and 9-fluorenylmethoxycarbonyl isothiocyanate (1.13 g) was added. After stirring at room temperature for 4 hr, piperidine (805 μl) was added. After stirring overnight at room temperature, the reaction mixture was concentrated under reduced pressure. The residue was partitioned by adding ethyl acetate and water. The organic layer was washed with saturated brine, dried over anhydrous magnesium sulfate, filtrated, and concentrated under reduced pressure. The residue was purified by column chromatography (ethyl acetate:n-hexane=1:1-4:1) to give the title compound (1.62 g).

1. stirringAfter stirring at room temperature for 4 hr
2. stirringAfter stirring overnight at room temperature
3. concentrationthe reaction mixture was concentrated under reduced pressure
4. customThe residue was partitioned
5. additionby adding ethyl acetate and water
6. washThe organic layer was washed with saturated brine
7. dry with materialdried over anhydrous magnesium sulfate
8. filtrationfiltrated
9. concentrationconcentrated under reduced pressure
10. customThe residue was purified by column chromatography (ethyl acetate:n-hexane=1:1-4:1)