反应详情

温度

85 °C

The product from Step B (744 mg, 1.40 mmol) was dissolved in methanesulfonic acid (6.0 mL) and heated to 85° C. for 50 min. After cooling in an ice-water bath, the reaction mixture was taken up in 2:3 MeCN—H2O (10 mL) and purified by reverse phase HPLC (C-18 column) to give the title compound (430 mg). LC/MS: m/z 491(M+H). 1H-NMR (d6-DMSO, 500 MHz): δ 5.40 (s, 2H), 6.96 (d, 1H), 7.20 (dd, 1H), 7.33 (t, 2H), 7.57 (d, 1H), 7.88 (d, 1H), 8.01 (s, 1H), 8.03 (s, 1H), 8.71 (d, 1H), 13.09 (s, 1H).

1. temperatureAfter cooling in an ice-water bath
2. custompurified by reverse phase HPLC (C-18 column)