反应详情

To a solution of 4-[4-(4,4,5,5-Tetramethyl-[1,3,2]dioxaborolan-2-yl)-pyrazol-1-yl]-piperidine-1-carboxylic acid tert-butyl ester (Intermediate B20) (1.5 eq, 1.095 mmol, 0.413 g) and 2M Na2CO3 (2.0 eq, 1.460 mmol, 0.730 ml) in DME (5 ml) is added (5″-Bromo-[2,2′;4′,3″]terpyridin-6′-yl)-methyl-amine (Example 2.1, step1) (1 eq, 0.730 mmol, 0.249 g) followed by [1,1′-Bis(diphenylphosphino)-ferrocene]dichloropalladium (II), complex with DCM (0.1 eq, 0.073 mmol, 0.059 g). The reaction mixture is heated using microwave radiation at 90° C. for 3 hours. The reaction mixture is dissolved in DCM and washed with water. The organic layer is washed with brine, dried over drying agent MgSO4, filtered and the organic solvent is reduced in vacuo. The crude residue is purified by flash chromatography (0-100% EtOAc in iso-hexane and up to 10% MeOH in EtOAc), to afford title compound.

1. temperatureThe reaction mixture is heated
2. customat 90° C.
3. customfor 3 hours
4. washwashed with water
5. washThe organic layer is washed with brine
6. customdried
7. dry with materialover drying agent MgSO4
8. filtrationfiltered
9. customThe crude residue is purified by flash chromatography (0-100% EtOAc in iso-hexane