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
- 40 °C
PROCEDURE
实验过程
(S)-2-(1-((5-(6-Methoxypyridin-2-yl)-7H-pyrrolo[2,3-d]pyrimidin-4-yl)amino)ethyl)-5-methyl-3-phenylpyrrolo[2,1-f][1,2,4]triazin-4(3H)-one (22 mg, 0.02 mmol) was dissolved in 440 μl acetonitrile. Sodium iodide (35 md, 0.24 mmol) and chlorotrimethylsilane (30 μl, 0.24 mmol) were added. The reaction mixture was stirred at 40° C. for 8 h. The mixture was poured into 10 mL of sodium bicarbonate solution and extracted twice with ethyl acetate. The organics were dried over sodium sulphate, filtered and concentrated under reduced pressure. The residue was purified using SP1® purification system (0% to 10%, dichloromethane-2-propanol) to give 4 mg (34% yield) of the title compound as a solid. Purity 93%.
WORKUP
后处理
- extractionextracted twice with ethyl acetate
- dry with materialThe organics were dried over sodium sulphate
- filtrationfiltered
- concentrationconcentrated under reduced pressure
- customThe residue was purified
- customSP1® purification system (0% to 10%, dichloromethane-2-propanol)