反应详情

温度

150 °C

Five reactions were set up with 6-bromo-4-nitro-2-(tetrahydro-2H-pyran-2-yl)-2H-indazole (500 mg, 1.53 mmol), [1,1′-bis(diphenylphosphino)ferrocene]dichloropalladium(II) (125 mg, 0.153 mmol), 1H-indol-4-ylboronic acid (370 mg, 2.3 mmol), saturated aqueous sodium hydrogen carbonate (3 ml) and isopropyl alcohol (12 ml) in each. They were all heated at 150° C. for 10 minutes in the microwave. The reaction mixtures were combined and water (250 ml) and ethyl acetate (250 ml) added. The mixture was filtered and the organic layer collected. The organic layer was washed with water followed by brine. The organic layer was dried over magnesium sulphate, filtered and solvent removed in vacuo. The residue was dissolved in dichloromethane and pre-absorbed onto silica. Purification was carried out using chromatography on silica eluting with 0-25% ethyl acetate in cyclohexane. The desired fractions were collected and combined and solvent removed in vacuo to give the title compound as a yellow solid (1.72 g).

1. customThe reaction mixtures
2. filtrationThe mixture was filtered
3. customthe organic layer collected
4. washThe organic layer was washed with water
5. dry with materialThe organic layer was dried over magnesium sulphate
6. filtrationfiltered
7. customsolvent removed in vacuo
8. dissolutionThe residue was dissolved in dichloromethane
9. custompre-absorbed onto silica
10. customPurification
11. customThe desired fractions were collected
12. customsolvent removed in vacuo