反应详情

温度

120 °C

Dissolve 1-(5-bromo-3-(trifluoromethyl)pyridin-2-yl)ethanone (2.67 g, 0.01 mol) in anhydrous DMF/H2O (30.0:0.3 mL) and degas the resulting solution with N2 for 10 minutes. Add Zn(CN)2 (1.17 g, 0.01 mol), Pd2(dba)3 (229 mg, 2.5 mol %) and DPPF (270 mg, 5 mol %). Purge the mixture with N2 for another 10 minutes and heat at 120° C. under N2 atmosphere for 45 minutes. Cool the reaction mixture to room temperature, dilute with water, extract with EtOAc (3×75 mL) and dry (MgSO4). Filter the dried extract and concentrate under vacuum to afford the crude product, which is purified by column chromatography to afford the title product as a yellow solid.

1. customdegas the resulting solution with N2 for 10 minutes
2. customPurge the mixture with N2 for another 10 minutes
3. temperatureCool the reaction mixture to room temperature
4. additiondilute with water
5. extractionextract with EtOAc (3×75 mL)
6. dry with materialdry (MgSO4)
7. filtrationFilter the dried
8. extractionextract
9. concentrationconcentrate under vacuum
10. customto afford the crude product, which
11. customis purified by column chromatography