反应详情

A solution of the product from Example 25 (55 mg, 0.104 mmol) in THF (1 ml) and 1N aq. NaOH (1 ml) was stirred in the dark at room temperature for 1.5 h. 1N aqueous HCl was added until pH 3, and the resulting mixture was extracted with EtOAc (2×2 ml). The combined organic layers were dried over Na2SO4, filtered and concentrated to give the title compound (53 mg, 99%). 1H NMR (300 MHz, DMSO-d6) δ 13.22 (br s, 1 H) 11.40 (d, J=2.21 Hz, 1 H) 10.02 (s, 1 H) 7.72-7.91 (m, 3 H) 7.68 (d, J=2.57 Hz, 1H) 7.49 (d, J=2.57 Hz, 1 H) 7.42 (dd, J=8.64, 2.39 Hz, 1 H) 7.21 (d, J=2.57 Hz, 1 H) 7.16 (d, J=16.18 Hz, 1 H) 5.64 (dd, J=7.72, 2.21 Hz, 1 H) 3.79 (s, 3 H) 3.04 (s, 3 H) 1.38 (s, 9 H).

1. extractionthe resulting mixture was extracted with EtOAc (2×2 ml)
2. dry with materialThe combined organic layers were dried over Na2SO4
3. filtrationfiltered
4. concentrationconcentrated