反应详情

A solution of Example 39H (0.050 g, 0.105 mmol), acetic anhydride (0.011 mL, 0.116 mmol), and pyridine (0.068 mL, 0.840 mmol) in methylene chloride (2 mL) was stirred at 25° C. for 4 hours. The solution was concentrated in vacuo and the residue was chromatographed on silica gel eluting with methylene chloride and 2.5% methanol in methylene chloride to give the desired product (0.046 g, 90%). 1H NMR (300 MHz, DMSO-d6): δ ppm 0.43 (m, 1H) 0.77 m, 7 H) 1.33 m, 1 H) 1.56 m, 3 H) 2.06 m, 4 H) 2.23 m, 1 H) 7.53 (m, 1 H) 7.66 m, 1 H) 7.77 m, 3 H) 8.16 m, 1 H) 8.29 m, 1 H) 10.38 m, 1 H) 13.84 (m, 1 H).

1. concentrationThe solution was concentrated in vacuo
2. customthe residue was chromatographed on silica gel eluting with methylene chloride and 2.5% methanol in methylene chloride