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
A suspension of 2-(4-hydroxy-2,6-dimethylphenyl)-4-(tetrahydropyran-4-ylmethyl)cyclopentane-1,3-dione (0.104 g, 0.00033 mol), 2,6-dichloroquinoline (0.065 g, 0.00033 mol) and potassium carbonate (0.140 g, 0.00101 mol) in anhydrous N,N-dimethylformamide (3 ml) is heated at 140° C. for 40 minutes under microwave irradiation. After cooling to room temperature the reaction mixture was quenched with 2M hydrochloric acid and extracted with ethyl acetate. The organic phase is separated, washed with distilled water then dried over anhydrous magnesium sulfate. The mixture is filtered, the filtrate is evaporated in vacuo and the residue is purified by preparative reverse phase HPLC to afford 2-[4-(6-chloroquinolin-2-yloxy)-2,6-dimethylphenyl]-4-(tetrahydropyran-4-ylmethyl)cyclopentane-1,3-dione.
WORKUP
后处理
- temperatureAfter cooling to room temperature the reaction mixture
- customwas quenched with 2M hydrochloric acid
- extractionextracted with ethyl acetate
- customThe organic phase is separated
- washwashed with distilled water
- dry with materialthen dried over anhydrous magnesium sulfate
- filtrationThe mixture is filtered
- customthe filtrate is evaporated in vacuo
- customthe residue is purified by preparative reverse phase HPLC