反应详情

温度

85 °C

The product of step B, compound 1-1-b, (3.2 g, 8.6 mmol) was dissolved in acetonitrile (100 mL), and treated with CAN (6.62 g, 12.1 mmol) and I2 (1.42 g, 5.6 mmol). The reaction mixture was stirred for 16 h at 85° C. The resulting mixture was concentrated, diluted with 50 mL of water, stirred for 20 min and filtered. The solid filtrate was dried under vacuum to provide the product, 1-1-c (3.6 g, 84%). 1H NMR (300 MHz, DMSO-d6) δ 6.22-6.24 (d, J=6.6, 1H), 7.22-7.39 (m, 11H), 7.55-7.74 (m, 1H), 8.07 (m, 1H), 8.47 (m, 1H), 8.71 (s, 1H), 10.49 (s, 1H). LC-MS 498[MH]+.

1. concentrationThe resulting mixture was concentrated
2. additiondiluted with 50 mL of water
3. stirringstirred for 20 min
4. filtrationfiltered
5. customThe solid filtrate was dried under vacuum