反应详情

温度

95 °C

To a solution of 5-chloro-N-(3,4-dimethoxyphenyl)thiazolo[5,4-d]pyrimidin-7-amine (140 mg, 0.433 mmol), methylpyrrolidine-3-carboxylate hydrochloride (107.7 mg, 0.65 mmol), X-Phos (115 mg, 0.24 mmol) and Cs2CO3 (580 mg, 1.78 mmol) in 60 mL of dry dioxane was added Pd2(dba)3 (60 mg, 0.065 mmol) in one portion at room temperature under nitrogen. Then the reaction mixture was degassed by nitrogen for 15 minutes. The mixture was then stirred at 95° C. under nitrogen for 24 hours. The solvent was evaporated at 40° C. at reduced pressure and the residue was purified by silica gel chromatography (silica gel 200-300 mesh, eluting a mixture of ethyl acetate and petroleum ether (2:1)) to give methyl 1-(7-(3,4-dimethoxyphenylamino)thiazolo[5,4-d]pyrimidin-5-yl)pyrrolidine-3-carboxylate (160 mg, 88.7%) as a yellow solid. LC-MS: 416.1 [M+H]+, tR=1.60 min.

1. customThen the reaction mixture was degassed by nitrogen for 15 minutes
2. customThe solvent was evaporated at 40° C. at reduced pressure
3. customthe residue was purified by silica gel chromatography (silica gel 200-300 mesh
4. washeluting
5. additiona mixture of ethyl acetate and petroleum ether (2:1))