반응 #543273

반응 방정식

6-chloro-3-[1-(4,6-difluoro-1-methyl-1H-indazol-5-yl)-ethyl]-imidazo[1,2-b]pyridazine

tributyl(1-ethoxyvinyl)stannane

N2

→

3-[1-(4,6-Difluoro-1-methyl-1H-indazol-5-yl)-ethyl]-6-(1-ethoxy-vinyl)-imidazo[1,2-b]pyridazine

용매

DMF

반응 조건

후처리

1. 1
   기타Then the reaction was quenched with water
2. 2
   추출extracted with EtOAc for three times
3. 3
   세척washed with KF solution and brine
4. 4
   건조dried over Na2SO4
5. 5
   기타Solvent was evaporated
6. 6
   기타the crude product (80 mg, 90%) was used in the next step without further purification

실험 절차

A solution of 6-chloro-3-[1-(4,6-difluoro-1-methyl-1H-indazol-5-yl)-ethyl]-imidazo[1,2-b]pyridazine (80 mg, 0.23 mmol) and tributyl(1-ethoxyvinyl)stannane (0.234 mL, 0.69 mmol) in 15 mL DMF was purged with N2 for 30 min and then tetrakis-(triphenylphosphine)-palladium (80 mg, 0.069 mmol) was added, and the solution was heated at 95° C. for overnight. Then the reaction was quenched with water, extracted with EtOAc for three times. The organic layers were combined, washed with KF solution and brine, dried over Na2SO4. Solvent was evaporated and the crude product (80 mg, 90%) was used in the next step without further purification. LCMS (method C): [MH]+=384.0, tR=4.67 min

출처