反应详情

The product from Example 55A (71 mg, 0.15 mmol) was treated with TFA (1 mL) at rt for 10 min, solvent removed and the mixture treated with saturated aqueous NaHCO3, and extracted with EtOAc (2×). The organic layer was dried over MgSO4, filtered and concentrated. The residue was purified by column chromatography using an Analogix® Intelliflash280™ (SiO2, 0-50% Hexane in ethyl acetate) to afford 51 mg (92%) of the title compound. 1H NMR (500 MHz, CDCl3) δ ppm 0.97 (t, J=7.32 Hz, 3 H) 1.36-1.47 (m, 2 H) 1.64 (s, 9 H) 1.67-1.77 (m, 2 H) 2.83 (dd, J=7.93 Hz, 2 H) 3.49 (brs, 2 H) 3.87 (s, 3 H) 6.76 (dd, J=8.54, 3.05 Hz, 1 H) 6.83 (d, J=8.54 Hz, 1 H) 7.54 (d, J=2.75 Hz, 1 H) 7.90 (s, 1 H); MS (DCI/NH4+) m/z 362 (M+H)+.

1. customsolvent removed
2. additionthe mixture treated with saturated aqueous NaHCO3
3. extractionextracted with EtOAc (2×)
4. dry with materialThe organic layer was dried over MgSO4
5. filtrationfiltered
6. concentrationconcentrated
7. customThe residue was purified by column chromatography