反应详情

温度

60 °C

16.3 g (43.6 mmol) of 2-[2-(3-bromocarbazol-9-yl)phenyl]propan-2-ol are dissolved in 1.2 l of degassed toluene, a suspension of 40 g of polyphosphoric acid and 28 ml of methanesulfonic acid is added, and the mixture is heated at 60° C. for 1 h. The batch is cooled, and water is added. A solid precipitates out and is dissolved in methylene chloride/THF (1:1). The solution is carefully rendered alkaline using 20% NaOH, the phases are separated and dried over MgSO4. The solid obtained is washed by stirring with heptane. Yield: 13.5 g (37 mmol), 87% of theory, purity according to 1H-NMR about 95%.

1. additionis added
2. temperatureThe batch is cooled
3. customA solid precipitates out and
4. dissolutionis dissolved in methylene chloride/THF (1:1)
5. customthe phases are separated
6. dry with materialdried over MgSO4
7. customThe solid obtained
8. washis washed