反应详情

A solution of the title compound from Step A (0.038 g, 0.131 mmol) in acetic acid (0.66 mL) was heated at 100° C. for 1 hour, then cooled to room temperature and concentrated under reduced pressure. The resulting residue was 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 (30-50% ethyl acetate in hexanes) provided the title compound: LCMS m/z 272.16 [M+H]+; 1H NMR (500 MHz, CDCl3) δ 9.06 (s, 1 H), 8.60 (d, J=2.7 Hz, 1 H), 8.03 (m, 1 H), 7.73 (dd, J=8.8, 4.8 Hz, 1 H), 7.30 (dd, J=8.6, 2.4 Hz, 1 H), 7.10-7.06 (m, 1 H), 3.59-3.55 (m, 1 H), 1.25-1.22 (m, 2 H), 0.83-0.80 (m, 2 H).

1. concentrationconcentrated under reduced pressure
2. additionThe resulting residue was diluted 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 (30-50% ethyl acetate in hexanes)