HRID601655
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
- 110 °C
PROCEDURE
实验过程
Under nitrogen atmosphere, 180 mg of N-methylisopropylamine, and 200 g of potassium carbonate were added at room temperature sequentially to 5 ml solution of dimethylsulfonamide with 63 g of 2-chloro-6-bromoquinoline, and the mixture was stirred at 110° C. for 4 hours. Water was added to the reaction solution, extracted with ethyl acetate. Ethyl acetate layer was washed with saturated saline solution, and dried with anhydrous sodium sulfate. The solvents were distilled outunder reduced pressure, and the residues were separated and purified by silicagel chromatography (hexane/ethyl acetate=3/1) to obtain 18 mg of the above compound as a white solid.
WORKUP
后处理
- extractionextracted with ethyl acetate
- washEthyl acetate layer was washed with saturated saline solution
- dry with materialdried with anhydrous sodium sulfate
- distillationThe solvents were distilled outunder reduced pressure
- customthe residues were separated
- custompurified by silicagel chromatography (hexane/ethyl acetate=3/1)