反应详情

温度

140 °C

A microwave vial was charged with a suspension of 10-bromo-2-(1-isopropyl-3-methyl-1H-1,2,4-triazol-5-yl)-5,6-dihydrobenzo[f]imidazo[1,2-d][1,4]oxazepine (0.200 mg, 0.515 mmol) in 2.0 ml THF/0.400 mL water. To this suspension was added potassium phosphate (330 mg, 0.0015 mol) and trimethylboroxine (0.14 ml, 1.00 mmol). The reaction suspension was degassed by bubbling nitrogen through the stirred mixture via a syringe. After several minutes the syringe was removed and Bis(ditertbutyl(4-dimethylaminophenyl)phosphine)dichloropalladium(II) (18 mg, 0.02 mmol) was added and the reaction vial was quickly sealed. The sealed vial was flash heated in a microwave at 140° C. for 40 minutes. The cooled reaction was diluted with EtOAc and the organic solution was washed with water×1, saline×1 and dried (Na2SO4) before concentration in vacuo. The crude residue was purified by preparative RP-HPLC to give 481. MS: (ESI+)=324.1

1. customThe reaction suspension was degassed
2. customby bubbling nitrogen through the stirred mixture via a syringe
3. customAfter several minutes the syringe was removed
4. customthe reaction vial was quickly sealed
5. customThe cooled reaction
6. washthe organic solution was washed with water×1, saline×1
7. dry with materialdried (Na2SO4)
8. concentrationbefore concentration in vacuo
9. customThe crude residue was purified by preparative RP-HPLC