HRID456091
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 95 °C
PROCEDURE
实验过程
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
WORKUP
后处理
- customThen the reaction was quenched with water
- extractionextracted with EtOAc for three times
- washwashed with KF solution and brine
- dry with materialdried over Na2SO4
- customSolvent was evaporated
- customthe crude product (80 mg, 90%) was used in the next step without further purification