反应详情

Under an atmospheric argon gas flow, 2,6-dibromoanthracene in an amount of 2.8 g (8.3 millimole), dried tetrahydrofuran (THF) in an amount of 200 milliliter and dried toluene in an amount of 200 milliliter were placed into a three necked-flask equipped with a cooling pipe and having a capacity of 1 liter and then, the resultant solution was cooled down to −30° C. Subsequently, n-butyllithium in an amount of 12 milliliter (19.1 millimole, 1.58 M hexane solution) was added slowly. Then, after adding trimethylsilylchloride in an amount of 2.4 milliliter (19.1 millimole, d=0.85) at a temperature of −70° C., the resultant solution was stirred at a room temperature for 1 hour. After completing the reaction, 100 milliliter of water was added and an organic layer was separated. The solution was dried with a use of sodium sulfate and then, the solvent was separated by distillation, and the residue was washed with a use of 100 milliliter of methanol and as a result, 1.7 g of pale yellow powder was obtained (the yield: 57%).

1. customequipped with a cooling pipe
2. additionwas added
3. customan organic layer was separated
4. dry with materialThe solution was dried with a use of sodium sulfate
5. customthe solvent was separated by distillation
6. washthe residue was washed with a use of 100 milliliter of methanol and as a result