反应详情

To a Schenk tube were charged compound tert-butyl 4-(7-(bis((2-(trimethylsilyl)ethoxy)methyl)amino)-6-bromo-3-(6-phenylpyridin-3-yl)pyrazolo[1,5-a]pyrimidin-5-yl)piperidine-1-carboxylate (81 mg, 0.1 mmol), Bu3SnCN (47 mg, 1.5 eq.), Pd(PPh3)4 (23 mg, 0.2 eq.), Bis(tri-t-butylphosphine)palladium (0) (10 mg, O2 eq.). The tube was evacuated and charged with Ar for three cycles. Dioxane (3 ml) was added; the tube was capped and heated at 160 C with stirring for one hour. After cooling, the mixture was diluted with EtOAc and washed with brine once. Organic layer separated, dried over MgSO4 and concentrated. The residue was purified on silica gel. Elution with EtOAc/hexane (0-25%) gave the desired title product (63 mg, 84%).

1. customThe tube was evacuated
2. additioncharged with Ar for three cycles
3. additionDioxane (3 ml) was added
4. customthe tube was capped
5. temperatureheated at 160 C
6. temperatureAfter cooling
7. additionthe mixture was diluted with EtOAc
8. washwashed with brine once
9. customOrganic layer separated
10. dry with materialdried over MgSO4
11. concentrationconcentrated
12. customThe residue was purified on silica gel
13. washElution with EtOAc/hexane (0-25%)