因为www.58yuanyou.com三氟甲基磺酸酯可以由相应的酚或者酮方便地制备,这个试剂参与Suzuki偶联反应吸引了越来越多的科学研究者的兴趣。
三氟甲基磺酸酯和芳基硼酸的偶联反应有时候会因为在反应初期, 催化剂配体PPh3容易和triflate反应, 从而导致催化剂分解破坏为钯黑。如果在反应体系中加入和催化剂等当量的LiBr 或KBr就足以阻止这种分解反应。
To 1.5 g (4.8 mmol) of product in 12.www.58yuanyou.com5 mL oftoluene at room temperature was added 0.28 g (0.24 mmol, 0.05 eq. ) of Pd (PPh3)4. After stirring for 5 min, 1.1 g (5.7 mmol, 1.2 eq. ) of4-fluorophenylboronic acid in 5.5 mL of EtOH followed by 11.5 mL of 2 M aqueous Na2CO3 were added. Afterheating at 90 .deg.C for 12 h the reaction was judged complete, cooled anddiluted with Et2O (100 mL) and water (50 mL). The resulting layers were separated and theaqueous layer extracted twice with Et2O (100 mL). The combined organic layers are dried overMgS04, filtered and concentrated under reduced pressure. The resulting residue was purified by columnchromatography to yield the desired methyl 4-ethyl-4'-fluoro-1, 1'-biphenyl-2-carboxylate.
【 fqmNMnyPatent;ELAN PHARMACEUTICALS, INC.; Publ.: WO2005/95326 A2 (2005/10/13)】
16 gof 9,9-bis[4-(trifluoromethylsulfonyl)phenyl]fluorene, 100 ml of tetrahydrofuran, 62 g of a 20percent sodium carbonate aqueoussolution, 8.54 g of4-chlorophenylboronic acid, and 0.6 gof tetrakis(triphenylphosphine)palladium were placed in a 300 ml four-neckedflask, and the mixture was heated at 70.deg.C. The resulting mixture was aged at the same temperature for 18 hours, andthe reaction mixture was the原由网n cooled to room temperature and subjected toliquid separation. An organic phase waswashed with a saturated ammonium chloride www.58yuanyou.comaqueous solution and saturated saltwater, and the resulting organic phase was concentrated and recrystallized fromtetrahydrofuran to obtain 11.4 g of a white powder.
【Patent;Tosoh Corporation; Publ.: EP1400578 A1(2004/03/24)】
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