反应详情

Compound 37 (26 mg, 70 μmol) was dissolved in THF (3 mL, dried with mol. siev.). To this solution was added NaH (60% in oil, 8.2 mg, 210 μmol) and the reaction was incubated for 10 min at ambient temperature. To the reaction mixture was then added compound 39 (17.6 mg, 61 μmol) followed by incubation at ambient temperature for 16 h. To the reaction was then added 0.1 M HCl (aq) and EtOAc, the phases separated and the aqueous phase extracted with another portion of EtOAc. The pooled organic phases were dried (MgSO4), filtered and concentrated in vacuo which gave a crude product which was further purified by flash-chromatography (Silica; DCM:MeOH) to afford the title compound (30 mg, 78%). LC/MS>95%, m/z (ESI+)=632 (MH+).

1. customthe phases separated
2. extractionthe aqueous phase extracted with another portion of EtOAc
3. dry with materialThe pooled organic phases were dried (MgSO4)
4. filtrationfiltered
5. concentrationconcentrated in vacuo which
6. customgave a crude product which
7. customwas further purified by flash-chromatography (Silica; DCM:MeOH)