反应详情

温度

120 °C

In a 4 mL microwave vial 2-chloro-7-cyclopentyl-7H-pyrrolo[2,3-d]pyrimidine-6-carboxylic acid dimethylamide (98 mg, 0.336 mmol), 3-(6-amino-pyridazine-3-carbonyl)-3,8-diaza-bicyclo[3.2.1]octane-8-carboxylic acid tert-butyl ester (112 mg, 0.336 mmol), BINAP (10.5 mg, 0.017 mmol), Cs2CO3 (164 mg, 0.504 mmol) and Pd(OAc)2 (3.8 mg, 0.017 mmol) were added together. The tube was capped and then purged with N2 three times. Dioxane (1.68 mL) was added and the capped tube was heated to 120° C. for 20 min in a microwave reactor. After cooling the reaction mixture was diluted with heptane resulting in the crude product precipitating out. The crude product was isolated by filtration, re-suspended in water and subjected to vigorous stirring and sonication. After re-isolating by filtration the product was purified by normal phase silica chromatography with a 0 to 20% MeOH/EtOAc gradient which gave a light tan solid (115 mg, 0.195 mmol). MS m/z 590.6 (M+H)+.

1. customThe tube was capped
2. custompurged with N2 three times
3. additionDioxane (1.68 mL) was added
4. temperatureAfter cooling the reaction mixture
5. additionwas diluted with heptane resulting in the crude product
6. customprecipitating out
7. customThe crude product was isolated by filtration
8. customsonication
9. customAfter re-isolating by filtration the product
10. customwas purified by normal phase silica chromatography with a 0 to 20% MeOH/EtOAc gradient which