HRID562808
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 solution of bromine (0.57 g) in acetic acid (2 mL) is added dropwise to a solution of 8-benzyloxy-3-methyl-1H-quinolin-2-one (0.94 g) and sodium acetate (0.96 g) in acetic acid (12 mL) at room temperature. The reaction mixture is stirred at room temperature for 3 hours, evaporated, the residue partitioned between water (5 mL) and ethyl acetate (5 mL), extracting a further 2× with ethyl acetate (5 mL). Combined organic extracts are dried over magnesium sulphate and purified by flash column chromatography on silica gel, eluting with 2% methanol in dichloromethane.
WORKUP
后处理
- customevaporated
- customthe residue partitioned between water (5 mL) and ethyl acetate (5 mL)
- extractionextracting a further 2× with ethyl acetate (5 mL)
- dry with materialCombined organic extracts are dried over magnesium sulphate
- custompurified by flash column chromatography on silica gel
- washeluting with 2% methanol in dichloromethane