反应详情

A mixture of 5-bromo-3-trifluoromethyl-pyridin-2-ylamine (11.5 g, 48 mmol) with 4-trifluormethylphenylboronic acid (9.97 g, 52 mmol), Pd(PPh3)4 (551 mg, 1 mol %) and 1 M aq. Na2CO3 soln. (111 mL, 111 mmol) in DME (250 mL) at reflux for 1 h. Poured on icewater, extracted with EtOAc, dried over Na2SO4 and concentrated. Purified by column chromatography (heptane/AcOEt 2:1), then triturated the collected solids with heptane and a few drops of ether, ultrasound sonication for 10 min, filtrated and dried in to give the product as a white crystalline solid (12.77 g, 87%). MS (ISP) 307.2 [(M+H)+].

1. additionPoured on icewater
2. extractionextracted with EtOAc
3. dry with materialdried over Na2SO4
4. concentrationconcentrated
5. customPurified by column chromatography (heptane/AcOEt 2:1)
6. customtriturated the collected solids
7. customwith heptane and a few drops of ether, ultrasound sonication for 10 min
8. filtrationfiltrated
9. customdried in