反应详情

To a solution of compound 8D was slowly added TFA (20 eq). The reaction mixture was stirred at rt till all the compound 8D was reacted (4-5 h, checked with LCMS). The solvent was removed with rotavapor at 25° C. More dichloromethane was added and the solvent was removed again. The same process repeated two more times. The residua were then transferred to a separatory funnel with EtOAc and washed with saturated aqueous NaHCO3. It was dried over sodium sulfate and filtered. Solvent was removed to give the title compound 9D in >85% yield. It was used for next step without further purification. LCMS (ESI) m/z 592.34 (MNa+), 570.44 (MH+). HPLC: tR=4.27 min.

1. customwas reacted (4-5 h, checked with LCMS)
2. customThe solvent was removed with rotavapor at 25° C
3. additionMore dichloromethane was added
4. customthe solvent was removed again
5. customThe residua were then transferred to a separatory funnel with EtOAc
6. washwashed with saturated aqueous NaHCO3
7. dry with materialIt was dried over sodium sulfate
8. filtrationfiltered
9. customSolvent was removed