反应详情

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 solution portionwise. The mixture was stirred at reflux for 30 min after the addition was complete. The mixture was cooled RT, and hexane (400 mL) was added. The mixture was stirred for 30 min and filtered, and the solids were washed with hexane to give the title compound (38 g, 88% yield). LRMS (M+H)+ Calcd.: 330.0; found 330.2.

1. temperatureto reflux (˜300 C)
2. temperatureat reflux for 30 min
3. additionafter the addition
4. stirringThe mixture was stirred for 30 min
5. filtrationfiltered
6. washthe solids were washed with hexane