反应详情

温度

100 °C

A mixture of 9-bromo-2-iodo-4,5-dihydro-6-oxa-1,3a-diazabenzo[e]azulene (200 mg, 0.512 mmol), 2-tributylstannanylpyridine (226 g, 0.614 mmol), Pd2(PPh3)2Cl2 (36 mg, 0.05 mmol) and copper iodide (29 mg, 0.15 mmol) in DMF (4 mL) was purged with nitrogen and then heated at 100° C. for 1 h using microwave irradiation. The reaction mixture was diluted with MeOH (20 mL) and then loaded onto an Isolute® SCX-2 cartridge which was washed with MeOH and the product eluted with 0.5M NH3/MeOH. The product containing fractions were combined and concentrated in vacuo. The resulting residue was purified by column chromatography (Si-PCC, gradient 0-8% MeOH in DCM followed by Si-PCC, gradient 0-7% MeOH in EtOAc) affording the title compound as a cream solid (140 mg, 80%). LCMS: RT 2.52 min [M+H]+ 341.8/343.8.

1. customwas purged with nitrogen
2. custommicrowave irradiation
3. additionThe reaction mixture was diluted with MeOH (20 mL)
4. washwas washed with MeOH
5. washthe product eluted with 0.5M NH3/MeOH
6. additionThe product containing fractions
7. concentrationconcentrated in vacuo
8. customThe resulting residue was purified by column chromatography (Si-PCC, gradient 0-8% MeOH in DCM followed by Si-PCC, gradient 0-7% MeOH in EtOAc)