反应详情

温度

300 °C

DOWTHERM A (450 mL) was heated to reflux (˜300° C.). A mixture of the product from Step 2 (49 g, 130 mmol) in DOWTHERM A (50 mL) was added to the heated Dowtherm A portionwise, and the mixture stirred at reflux for 30 minutes after addition was complete. The mixture was cooled to RT; hexane (400 mL) was added; and the mixture was stirred for 30 minutes, filtered, and the solids washed with hexane to give the title compound (38 g). LRMS (M+H)+ Calcd.: 330.0; found 330.2.

1. temperatureat reflux for 30 minutes
2. additionafter addition
3. temperatureThe mixture was cooled to RT
4. stirringand the mixture was stirred for 30 minutes
5. filtrationfiltered
6. washthe solids washed with hexane