HRID1750123
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
PROCEDURE
实验过程
A mixture of intermediate 38 (253 mg, 1.68 mmol), 1,4-dibromobutane (0.6 mL, 5.04 mmol) and anhydrous K2CO3 (232 mg, 1.68 mmol) was dissolved in EtOH and the solution was heated to reflux overnight. The solution was diluted with water and extracted with EtOAc. The combined organic layers were washed with saturated NaHCO3, brine, dried over anhydrous Na2SO4, concentrated in vacuo and purified by flash chromatography on silica gel column (elution with PE/EtOAc=4:1) to give 7-(4-bromobutoxy)quinolin-2(1H)-one (intermediate 48) (120 mg, 25%) as a yellow solid.
WORKUP
后处理
- temperaturethe solution was heated
- temperatureto reflux overnight
- extractionextracted with EtOAc
- washThe combined organic layers were washed with saturated NaHCO3, brine
- dry with materialdried over anhydrous Na2SO4
- concentrationconcentrated in vacuo
- custompurified by flash chromatography on silica gel column (elution with PE/EtOAc=4:1)