反应详情

温度

150 °C

To a suspension of 1-[3-(7-Chloro-imidazo[1,2-a]pyridin-3-yl)-phenyl]-3-(2,2,2-trifluoro-ethyl)-urea (0.1 g, 0.27 mmol), tributyl-(1-ethoxy-vinyl)-stannane (0.091 ml, 0.27 mmol, 1 equiv), lithium chloride (0.034 g, 0.81 mmol, 3 equiv) in acetonitrile (4 ml) was added tetrakis(triphenylphosphine)palladium(0) (0.031 g, 27.2 μmol, 0.1 equiv). The reaction mixture was degassed by bubbling through N2, heated in the microwave at 150° C. for 20 min and filtered through a glass microfibre filter. To the filtrate was added 2N HCl (3 ml) and the mixture stirred vigorously for 2 h at room temperature, neutralised with saturated aqueous NaHCO3, extracted with CH2Cl2, the organics combined dried (MgSO4) and the solvent removed in vacuo. The residue was purified by preparative LC-MS to give the desired product as a yellow solid. MS: [M+H]+ 377

1. customThe reaction mixture was degassed
2. customby bubbling through N2
3. filtrationfiltered through a glass microfibre
4. filtrationfilter
5. additionTo the filtrate was added 2N HCl (3 ml)
6. extractionextracted with CH2Cl2
7. dry with materialthe organics combined dried (MgSO4)
8. customthe solvent removed in vacuo
9. customThe residue was purified by preparative LC-MS