反应详情

温度

90 °C

To a solution of tert-butyl 3-aminoazepane-1-carboxylate (1 g, 4.7 mmol), 4-chloro-7-tosyl-7H-pyrrolo[2,3-d]pyrimidine (3.1 g, 5.1 mmol) in DMF (10 mL) was added DIEA (1.2 mL, 7.0 mmol) and the reaction mixture was heated to 90° C. for 3 h. The reaction was cooled to rt and diluted with ice cooled water (50 mL). The mixture was extracted with EtOAc (3×100 mL), the EtOAc layers were combined, dried over Na2SO4 and evaporated in vacuo to give the crude product that was purified by column chromatography (silica gel, gradient 0-20% EtOAc hexane) to afford the titled intermediate (1.4 g, 89%). LC-MS: m/z [M+1]=486.

1. temperatureThe reaction was cooled to rt
2. additiondiluted with ice
3. extractionThe mixture was extracted with EtOAc (3×100 mL)
4. dry with materialdried over Na2SO4
5. customevaporated in vacuo
6. customto give the crude product that
7. customwas purified by column chromatography (silica gel, gradient 0-20% EtOAc hexane)