反应详情

Intermediate 61H (825 mg, 1.67 mmol) was dried azeotropically with toluene (2×). The residue was taken up in 15% TFA in CH2Cl2 (10 mL) and stirred at rt for 5 h. Toluene (10 mL) was added and solvent was removed under vacuum. The product was purified by reverse phase HPLC (Phenomenex Luna 30×100 mm S5 C18, 10 min. grad, 25 mL/min, 20-100% B solvent, A=10% MeOH/water+0.1% TFA, B=90% MeOH/Water+0.1% TFA, 4 injections). Solvent was reduced to ˜10% volume and the product was then extracted into EtOAc, washed with sat. aqueous NaHCO3, dried over MgSO4 and filtered. Solvents were removed to provide the title compound (371 mg): MS (ES) m/z 394.53 [M+H]+

1. customsolvent was removed under vacuum
2. customThe product was purified by reverse phase HPLC (Phenomenex Luna 30×100 mm S5 C18, 10 min.
3. extractionthe product was then extracted into EtOAc
4. washwashed with sat. aqueous NaHCO3
5. dry with materialdried over MgSO4
6. filtrationfiltered
7. customSolvents were removed