HRID456091

反应详情

EQUATION

反应方程式

HRID 456091 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. customThen the reaction was quenched with water
  2. extractionextracted with EtOAc for three times
  3. washwashed with KF solution and brine
  4. dry with materialdried over Na2SO4
  5. customSolvent was evaporated
  6. customthe crude product (80 mg, 90%) was used in the next step without further purification