反应详情

温度

80 °C

1-(Phenylsulfonyl)-6-(4,4,6,6-tetramethyl-1,3,2-dioxaborinan-2-yl)-1H-indazol-4-amine (2 g, 4.84 mmol), 4-bromo-1H-pyrrolo[2,3-b]pyridine (0.953 g, 4.84 mmol), Pd(dppf)Cl2 (0.708 g, 0.968 mmol) and Tripotassium phosphate (3.08 g, 14.52 mmol) were divided between 2× microwave vials and dissolved in 1,4-dioxane (24 ml) and water (8.00 ml); 12 ml dioxane and 4 ml water in each vial. The mixtures were heated in the microwave at 80° C. for 20 min. Solvent was removed in vacuo and the residue was partitioned between DCM (100 ml) and water (100 ml). The organic layer was collected using a hydrophobic frit and the solvent removed in vacuo. DCM was added to dissolve the crude residue but a suspension resulted. The yellow solid was filtered off and dried in a vacuum oven for 30 mins to afford the title compound (919 mg). The filtrate was concentrated in vacuo and dissolved in DCM, then applied to the top of a 50 g silica SPE cartridge. This was eluted with 0-100% EtOAc/DCM over 60 mins on the FlashMaster II. The product-containing fractions were combined to give a further portion of the title compound as a yellow solid (220 mg).

1. customSolvent was removed in vacuo
2. customthe residue was partitioned between DCM (100 ml) and water (100 ml)
3. customThe organic layer was collected
4. customthe solvent removed in vacuo
5. additionDCM was added
6. dissolutionto dissolve the crude residue
7. customa suspension resulted
8. filtrationThe yellow solid was filtered off
9. customdried in a vacuum oven for 30 mins