反应详情

温度

90 °C

A solution of 5-chloro-1-(p-tolylsulfonyl)-3-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)pyrrolo[2,3-b]pyridine (2.41 g, 5.60 mmol) and tert-butyl (3S)-3-[(2-chloro-5-fluoro-pyrimidin-4-yl)amino]pyrrolidine-1-carboxylate, 7a, (1.69 g, 5.30 mmol) in DME (34 mL) and 2M Na2CO3 (8.5 mL) was degassed with nitrogen (5 min) then treated with Pd(PPh3)4 (0.31 g, 0.27 mmol) then heated at 90° C. overnight. The resulting dark solution was filtered through florisil, washed with EtOAc then concentrated in vacuo. The resulting residue was purified by silica-gel chromatography (0-100%) petroleum ether: EtOAc gradient. Removal of the solvent under reduced pressure afforded 1.33 g (42% yield) of a white solid after vacuum drying.

1. filtrationThe resulting dark solution was filtered through florisil
2. washwashed with EtOAc
3. concentrationthen concentrated in vacuo
4. customThe resulting residue was purified by silica-gel chromatography (0-100%) petroleum ether
5. customRemoval of the solvent under reduced pressure