反应详情

Compound 217 (0.094 g, 0.15 mmol) was combined with 10 mL of methanol and 4 mL of 1N HCl. The solution was stirred at room temperature overnight. The solution was concentrated under vacuum and the residue obtained was purified on CombiFlash column (dry loaded), eluting with a gradient of 2% methanol/0.1% NH4OH (˜28% in water)/DCM to 10% methanol/0.5% NH4OH (˜28% in water)/DCM. The fractions containing the product were combined and concentrated under vacuum to give a yellow solid. The solid was partially dissolved in methanol and then collected on filter paper. Washed the solid off of the filter paper with DCM/methanol through a fritted funnel and then concentrated under vacuum to give compound 213 (0.065 g, 85% yield) as a yellow solid. 1H-NMR (500 MHz, DMSO-d6) δ 9.92 (1 H, s), 9.33 (1 H, s), 8.22 (1 H, d, J=5.1 Hz), 8.10 (1 H, d, J=4.9 Hz), 8.04 (1 H, d, J=2.9 Hz), 8.02 (1 H, d, J=9.0 Hz), 7.46 (1 H, dd, J=9.0, 2.9 Hz), 5.95-6.05 (1 H, m), 4.43 (1 H, t, J=5.4 Hz), 3.54 (2 H, q, J=6.1 Hz), 3.12-3.19 (4 H, m), 2.55-2.65 (6 H, m), 2.45 (2 H, t, J=6.4 Hz), 1.98-2.08 (4 H, m), 1.65-1.75 (2 H, m) ppm; LCMS-ESI (POS), M/Z, M+1: Found 493.1.

1. concentrationThe solution was concentrated under vacuum
2. customthe residue obtained
3. customwas purified on CombiFlash column (dry loaded)
4. washeluting with a gradient of 2% methanol/0.1% NH4OH (˜28% in water)/DCM to 10% methanol/0.5% NH4OH (˜28% in water)/DCM
5. additionThe fractions containing the product
6. concentrationconcentrated under vacuum
7. customto give a yellow solid
8. customcollected
9. filtrationon filter paper
10. washWashed the solid off of the filter paper with DCM/methanol through a fritted funnel
11. concentrationconcentrated under vacuum