反应详情

5-Bromo-N-(2-(dimethylamino)ethyl)isoquinolin-1-amine (0.068 g, 0.2 mmol) was added to a microwave vial equipped with a stirbar, along with 1-(2-hydroxy-2-methylpropyl)-5-methyl-3-oxo-2-phenyl-N-(4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)phenyl)-2,3-dihydro-1H-pyrazole-4-carboxamide (0.2 g, 0.3 mmol). Then 1,4-Dioxane (3 ml, 35 mmol) was added into the mixture, followed by 2M K2CO3 (0.5 ml). Then Fibrecat (2.93% Pd, 0.010 g) was added to the mixture. The vial was capped, then placed into CEM Microwave for 10 minutes at 120° C. with 80 Watts of power supplied through Powermax feature. The mixture was diluted with DCM and water, then collected the organic layer by extracting with DCM (3×10 ml). Combined organics, dried over Na2SO4, filtered and concentrated in-vacuo. The crude was purified by ISCO Amino-propyl chromatography using MeOH/DCM as the eluent. This gave the title compounds as a tan amorphous solid (85 mg). MS (ESI pos. ion) m/z: 579 (MH+). Calc'd exact mass for C34H38N6O3: 578.

1. customThe vial was capped
2. customcollected the organic layer
3. extractionby extracting with DCM (3×10 ml)
4. dry with materialCombined organics, dried over Na2SO4
5. filtrationfiltered
6. concentrationconcentrated in-vacuo
7. customThe crude was purified by ISCO Amino-propyl chromatography