反应详情

A solution of the title compound from Step D (0.070 g, 0.20 mmol) in acetic acid (1.0 mL) was heated at 100° C. for 1 hour, and then cooled to room temperature. The resulting mixture was concentrated under reduced pressure, diluted with ethyl acetate, washed sequentially with aqueous 1 N sodium hydroxide solution and brine, dried over magnesium sulfate, filtered and concentrated. Purification by flash chromatography on silica gel (50-80% ethyl acetated in hexanes) provided the title compound: LCMS m/z 330.04 [M+H]+; 1H NMR (500 MHz, CDCl3) δ 9.09 (s, 1 H), 8.87 (s, 1 H), 8.44 (d, J=1.8 Hz, 1 H), 7.58 (dd, J=10.3, 7.3 Hz, 1 H), 7.40 (dd, J=9.7, 7.0 Hz, 1 H), 3.59-3.58 (m, 1 H), 2.89 (br s, 1 H), 1.69 (s, 6 H), 1.22-1.19 (m, 2 H), 0.79-0.78 (m, 2 H).

1. concentrationThe resulting mixture was concentrated under reduced pressure
2. additiondiluted with ethyl acetate
3. washwashed sequentially with aqueous 1 N sodium hydroxide solution and brine
4. dry with materialdried over magnesium sulfate
5. filtrationfiltered
6. concentrationconcentrated
7. customPurification by flash chromatography on silica gel (50-80% ethyl acetated in hexanes)