反应详情

A mixture of 2-[4-(4-morpholin-4-yl-2-(tributylstannanyl)thieno[3,2-d]pyrimidin-6-ylmethyl)piperazin-1-yl]isobutyramide (0.241 g, 0.35 mmol), 1-benzenesulfonyl-4-bromo-2-ethyl-1H-pyrrolo[2,3-c]pyridine (0.14 g, 0.38 mmol), copper(I) 2-thiophene carboxylate (0.01 g, 0.069 mmol) and Pd(PPh3)4 (0.040 g, 0.035 mmol) in dioxane (3 mL) was subjected to microwave irradiation at 150° C. for 20 min. The reaction mixture was loaded onto an Isolute® SCX-2 cartridge. The cartridge was washed with MeOH and the desired product was eluted using 2 M NH3 in MeOH. The eluent was concentrated in vacuo and the residue was purified by flash chromatography (Si—PPC, MEOH:DCM, gradient 0:100 to 20:80) to give 2-{4-[2-(1-benzenesulfonyl-2-ethyl-1H-pyrrolo[2,3-c]pyridin-4-yl)-4-morpholin-4-ylthieno[3,2-d]pyrimidin-6-ylmethyl]piperazin-1-yl}isobutyramide as a yellow foam (0.15 g, 64%). LCMS (Method A): RT=3.53min, [M+H]+ 689.2

1. customirradiation at 150° C. for 20 min
2. washThe cartridge was washed with MeOH
3. washthe desired product was eluted
4. concentrationThe eluent was concentrated in vacuo
5. customthe residue was purified by flash chromatography (Si—PPC, MEOH:DCM, gradient 0:100 to 20:80)