反应详情

A solution of 3-bromo-5-methyl-1H-pyrazolo[3,4-c]pyridine (2.13 g, 10.04 mmol), tri-butyl(1-ethoxyvinyl)tin (6.78 mL, 20.09 mmol) and PdCl2(PPh3)2 (0.705 mg, 1 mmol) in DMF (12.6 mL) was heated at 80° C. overnight under argon atmosphere. Then concentrated under reduced pressure and diluted with EtOAc. HCl (2N) was added, the layers were separated and the aqueous layer was basified by addition of NaHCO3 (1N in water) and extracted with EtOAc (3×). The combined organic extracts were dried (Na2SO4), filtered and concentrated. The yellow oil thus obtained was used without further purification in the next step. TLC, Rf (c-hexane/EtOAC 1:1)=0.05; MS (UPLC/MS): 176 [M+H]+, 174 [M−H]−.

1. concentrationThen concentrated under reduced pressure
2. additiondiluted with EtOAc
3. additionHCl (2N) was added
4. customthe layers were separated
5. additionthe aqueous layer was basified by addition of NaHCO3 (1N in water)
6. extractionextracted with EtOAc (3×)
7. dry with materialThe combined organic extracts were dried (Na2SO4)
8. filtrationfiltered
9. concentrationconcentrated
10. customThe yellow oil thus obtained
11. customwas used without further purification in the next step