反应详情

温度

82.5 °C

Stir 6-fluoro-2-methyl-4H-3-thia-4,9-diaza-benzo[f]azulen-10-ylamine hydrochloride (82.5 g, 0.291 mol) as a suspension in deionized water (2475 mL) at ambient temperature. Add EtOH (830 mL) and stir for 15 minutes. Add potassium carbonate (301 g, 2.18 mol) with stirring and heat to gentle reflux (80-85° C.) for 3-4 days. Allow cooling to ambient temperature. Filter the product and rinse with 3:1/water:EtOH, then water. Dry the solid at 50-60° C. to give 55.2 g (76%) the title compound: 1H NMR (400 MHz, DMSO-d6) δ 9.18 (bs, 1H), 9.00 (bs, 1H), 6.90 (m, 1H), 6.73 (m, 1H), 6.60 (m, 2H), 2.24 (s, 3H). HRMS (ES) exact mass M+H calcd for C12H9FN2OS 249.0498; found 249.0488.

1. temperatureheat
2. temperatureAllow cooling to ambient temperature
3. filtrationFilter the product
4. washrinse with 3:1/water
5. customDry the solid at 50-60° C.