反应详情

Compound 5 (4.07 g, 12.79 mmol) was mixed with 4,4′-dimethoxytrityl chloride (4.56 g, 13.46 mmol) and dried over P2O5 under reduced pressure. The residue was dissolved in anhydrous pyridine (43 mL) and stirred at room temperature for 6 hours under an atmosphere of argon. The mixture was quenched with methanol (3 mL). The reaction mixture was diluted with EtOAc (200 mL), washed with aqueous NaHCO3 (saturated, 300 mL) and brine (200 mL) then dried over Na2SO4, filtered and concentrated. The residue obtained was purified by silica gel column chromatography (eluted first with 70% EtOAc in hexanes and then increasing the polarity) to yield Compound 6 (7.1 g, 89%). ES MS m/z 643.2 [M+Na]+.

1. dry with materialdried over P2O5 under reduced pressure
2. dissolutionThe residue was dissolved in anhydrous pyridine (43 mL)
3. customThe mixture was quenched with methanol (3 mL)
4. additionThe reaction mixture was diluted with EtOAc (200 mL)
5. washwashed with aqueous NaHCO3 (saturated, 300 mL) and brine (200 mL)
6. dry with materialthen dried over Na2SO4
7. filtrationfiltered
8. concentrationconcentrated
9. customThe residue obtained
10. customwas purified by silica gel column chromatography (
11. washeluted first with 70% EtOAc in hexanes
12. temperatureincreasing the polarity)