HRID244768

反应详情

EQUATION

反应方程式

HRID 244768 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customevaporated
  2. customthe residue partitioned between water (5 mL) and ethyl acetate (5 mL)
  3. extractionextracting a further 2× with ethyl acetate (5 mL)
  4. dry with materialCombined organic extracts are dried over magnesium sulphate
  5. custompurified by flash column chromatography on silica gel
  6. washeluting with 2% methanol in dichloromethane