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
- 100 °C
PROCEDURE
实验过程
100 mg (0.19 mmol) of N-[4-({3-bromo-1-[(4-methylphenyl)sulfonyl]-1H-pyrrolo[2,3-b]pyridin-4-yl}oxy)-3-fluorophenyl]acetamide are dissolved in dioxane (2.5 ml). The solution is degassed and vented with argon. 0.29 ml (0.58 mmol) of a 2M solution of dimethylzinc in toluene and 7.9 mg (0.01 mmol) of [1,1′-bis(diphenylphosphino)ferrocene]palladium(II) chloride/methylene dichloride complex are added, and the mixture is heated at 100° C. for 2.5 hours. The mixture is allowed to cool to RT, acetic acid and 1M hydrochloric acid are added and the aqueous phase is extracted with ethyl acetate. The combined organic phases are dried over sodium sulfate and the solvent is removed under reduced pressure. The residue is purified by preparative HPLC.
WORKUP
后处理
- customThe solution is degassed
- temperatureto cool to RT
- extractionthe aqueous phase is extracted with ethyl acetate
- dry with materialThe combined organic phases are dried over sodium sulfate
- customthe solvent is removed under reduced pressure
- customThe residue is purified by preparative HPLC