反应详情

温度

100 °C

35.51 g (234.9 mmol) of methyl anthranilate are dissolved in 500 ml of toluene and degassed well. 52 g (213 mmol) of 1-bromocarbazole, 2.1 g (10.7 mmol) of 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene, 1.19 g (5.34 mmol) of Pd(OAc)2 and 76.5 g (234.9 mmol) of Cs2CO3 are added, and the mixture is then degassed and stirred at 100° C. under a protective-gas atmosphere for 24 h. The solids are subsequently filtered off via Celite, and the organic phase is washed with water, dried over MgSO4 and evaporated. The crude product is washed by stirring with hot heptane, giving 57.4 g (108 mmol), 86% of theory, purity according to HPLC 86%.

1. customdegassed well
2. customthe mixture is then degassed
3. filtrationThe solids are subsequently filtered off via Celite
4. washthe organic phase is washed with water
5. dry with materialdried over MgSO4
6. customevaporated
7. washThe crude product is washed
8. stirringby stirring with hot heptane
9. customgiving 57.4 g (108 mmol), 86% of theory, purity