反应详情

温度

50 °C

The product from Step (c) above (2.6 g, 11.4 mmol) was dissolved in acetonitrile (20 mL) and diketene (0.86 mL, 11.2 mmol) was added in portions over min, then the solution was sealed and heated to 50° C. overnight. The reaction mixture was then cooled, filtered and the filtrate was concentrated to give the title compound as a dark tan solid (2.6 g, 73%). NMR 1H NMR (400 MHz, DMSO-D6) δ 10.86 (s, 1H), 10.32 (s, 1H), 8.25-8.20 (m, 2H), 7.75 (dd, J=8.9, 2.0, 1H), 3.59 (s, 2H), 2.63 (s, 3H), 2.22 (s, 3H), 3.18 (s, 3H) MS m/z 317.0 [M+H]+

1. customthe solution was sealed
2. temperatureThe reaction mixture was then cooled
3. filtrationfiltered
4. concentrationthe filtrate was concentrated