反应详情

2,4-Dimethoxy-pyrimidine-5-boronic acid (2.05 g, 11.21 mmol) was dissolved in degassed n-PrOH (80 ml) and then 3-iodo-pyridazine (Prep 119, 2.1 g, 10.19 mmol), Na2CO3 (3.24 g, 30.57 mmol), PPh3 (890 mg, 3.40 mmol) and Pd(OAc)2 (180 mg, 0.8 mmol) were added. The suspension was stirred at reflux for 5 hours. The solvent was evaporated under vacuum and the crude was partitioned between water and ethyl acetate. The organic phase washed with brine, dried (Na2SO4) and evaporated. The residue was triturated with iPrOH to afford 750 mg of the title compound as a white powder (34% yield).

1. temperatureat reflux for 5 hours
2. customThe solvent was evaporated under vacuum
3. customthe crude was partitioned between water and ethyl acetate
4. washThe organic phase washed with brine
5. dry with materialdried (Na2SO4)
6. customevaporated
7. customThe residue was triturated with iPrOH