反应详情

温度

300 °C

DOWTHERM A (0.19 M) was heated to reflux (˜300° C.). A mixture of the product 113 in DOWTHERM A (2.5 M) was added to the heated DOWTHERM A solution portionwise. The mixture was stirred at reflux for 1 h after the addition was complete. The mixture was cooled to RT, filtered, and the solid was washed with hexane to give the title compound 114 (86%). 1H NMR (DMSO-d6) (ppm) 11.69 (s, 1H), 8.19 (s, 1H), 7.82 (m, 2H), 7.59 (m, 3H), 7.35 (s, 1H), 6.33 (s, 1H), 3.96 (s, 3H).

1. temperatureat reflux for 1 h
2. additionafter the addition
3. temperatureThe mixture was cooled to RT
4. filtrationfiltered
5. washthe solid was washed with hexane