反应详情

温度

130 °C

3-Hydroxy-5-iodo-3-phenyl-1,3-dihydro-indol-2-one (130 mg, 0.370 mmol), 3,5-dimethyl-4-isoxazolylboronic acid (104 mg, 0.740 mmol), sodium carbonate (108 mg, 1.025 mmol), Pd(dppf)Cl2 (57 mg, 78 mmol) and lithium chloride (114.5 mg, 2.700 mmol) are added to a microwave vial. Dioxane/water (2:1, 3 mL) is added. The mixture is flushed with argon and the vessel heated at 130° C. for 1 h. The reaction mixture is diluted with water and dcm then extracted with dcm. The organic layer is dried with Na2SO4, filtered and concentrated under reduced pressure. The residue is dissolved in DMSO, filtered and purified with the acidic (formic acid) RP HPLC system. The product containing fractions are concentrated under reduced pressure. Dissolved in DMSO, aliquoted and freeze dried. Once more freeze dried with acetonitril: water. This afforded the desired product.

1. customThe mixture is flushed with argon
2. additionThe reaction mixture is diluted with water and dcm
3. extractionthen extracted with dcm
4. dry with materialThe organic layer is dried with Na2SO4
5. filtrationfiltered
6. concentrationconcentrated under reduced pressure
7. dissolutionThe residue is dissolved in DMSO
8. filtrationfiltered
9. custompurified with the acidic (formic acid) RP HPLC system
10. additionThe product containing fractions
11. concentrationare concentrated under reduced pressure
12. dissolutionDissolved in DMSO
13. customfreeze dried
14. dry with materialOnce more freeze dried with acetonitril