反应详情

温度

150 °C

A microwave vial was charged with a solution 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, 0.466 mmol) in 1.4 ml DMF. To this solution was added zinc cyanide (160 mg, 1.4 mmol). The reaction mixture 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) (66 mg, 0.093 mmol) was added and the reaction vial was quickly sealed. The sealed vial was flash heated in a microwave at 150° C. for 30 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 455. MS: (ESI+)=335.1

1. customThe reaction mixture 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