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
- 140 °C
PROCEDURE
实验过程
Potassium carbonate (115 mg) and 6-chloro-5-fluoro-2-(quinolin-6-ylamino)nicotinonitrile (50 mg) were added to a tube containing a 1,4-dioxane (2 ml) solution containing (R)-2-(2-aminopropyl)isoindoline-1,3-dione (52 mg) and the tube was sealed, followed by stirring with heating at 140° C. for 13 hours. The reaction solution was adjusted to room temperature, and a saturated aqueous sodium hydrogen carbonate solution was added, followed by extraction with ethyl acetate. The organic layer was dried over anhydrous sodium sulfate. Subsequently, the solvent was distilled away under reduced pressure, the obtained residue was purified by silica gel chromatography (n-hexane:ethyl acetate=3:2), and a yellow solid of (R)-6-((1-(1,3-dioxoisoindolin-2-yl)propan-2-yl)amino)-5-fluoro-2-(quinolin-6-ylamino)nicotinonitrile (57 mg) was thus obtained.
WORKUP
后处理
- customthe tube was sealed
- customwas adjusted to room temperature
- extractionfollowed by extraction with ethyl acetate
- dry with materialThe organic layer was dried over anhydrous sodium sulfate
- distillationSubsequently, the solvent was distilled away under reduced pressure
- customthe obtained residue was purified by silica gel chromatography (n-hexane:ethyl acetate=3:2)