反应详情

温度

85 °C

To 8-fluoro-1-oxo-2,5-dihydro-1H-pyrido[4,3-b]indole-4-carbonitrile (23.5 g, 103 mmol) in dioxane (235 mL) was added POCl3 (95 g, 621 mmol) at 85° C. The reaction mixture was left to stir at 85° C. for 3 h, cooled to 0° C., and treated with MTBE. The reaction mixture was filtered, and washed with MTBE. The solid was treated with isopropanol, warm to 45° C. for 2 h, cooled to room temperature, filtered, washed with MTBE, and dried to afford the title compound as an HCl salt. 1H NMR (600 MHz, CD3COCD3) δ 8.68 (s, 1H); 8.15 (dd, 1H); 7.78 (dd, 1H); 7.48 (dt, 1H). LRMS (APCI) calc'd for (C12H5ClFN3) [M+H]+, 246.0. found 246.0.

1. waitThe reaction mixture was left
2. temperaturecooled to 0° C.
3. filtrationThe reaction mixture was filtered
4. washwashed with MTBE
5. additionThe solid was treated with isopropanol
6. temperaturewarm to 45° C. for 2 h
7. temperaturecooled to room temperature
8. filtrationfiltered
9. washwashed with MTBE
10. customdried