反应详情

温度

150 °C

A 20 mL microwave vial was charged with a suspension of 2-[1-(9-methyl-6-morpholin-4-yl-2-(tributylstannanyl)-9H-purin-8-ylmethyl)piperidin-4-yl]propan-2-ol (0.5 g, 0.75 mmol), 1-benzenesulfonyl-4-bromo-1H-pyrrolo[2,3-c]pyridine (0.29 g, 0.83 mmol), CuTC (0.029 g, 0.015 mmol) and Pd(PPh3)4 (0.087 g, 0.075 mmol) in dioxane (8 mL). The reaction mixture was heated in a microwave for 30 min at 150° C. The cooled reaction mixture was loaded onto an SCX-2 cartridge. The cartridge was washed with 3 volumes of MeOH, then the product was recovered eluting with 2N ammonia in MeOH. The solution was concentrated and the residue loaded onto a 40g SiO2 column and purified by flash chromatography (Si—PCC; 40g SiO2 column, 0% to 6% MeOH in DCM) to give 2-{1-[2-(1-Benzenesulfonyl-2-methyl-1H-pyrrolo[2,3-c]pyridin-4-yl)-9-methyl-6-morpholin-4-yl-9H-purin-8-ylmethyl]piperidin-4-yl}propan-2-ol as white foam (0.414 g, 86%). LCMS (Method A): RT=3.24 min, [M+H]+ 645.3

1. customThe cooled reaction mixture
2. washThe cartridge was washed with 3 volumes of MeOH
3. customthe product was recovered
4. washeluting with 2N ammonia in MeOH
5. concentrationThe solution was concentrated
6. custompurified by flash chromatography (Si—PCC; 40g SiO2 column, 0% to 6% MeOH in DCM)