HRID2393084

反应详情

EQUATION

反应方程式

HRID 2393084 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
45 °C

PROCEDURE

实验过程

A solution of 8-methoxy-2-methylquinoline (1.0 g) in methanol (30 ml) was treated at room temperature with bromine (0.31 ml). The mixture was heated at 45° C. for 2 hours and the reaction quenched with 5% aqueous sodium metabisulphite (50 ml). The solution was basified with 25% aqueous sodium hydroxide to pH13 and the product extracted with ethyl acetate (2×100 ml). The extracts were combined, dried over magnesium sulphate, filtered and the filtrate evaporated in vacuo. The residue was dissolved in ethyl acetate and passed through a silica pad. The solution was evaporated in vacuo to yield the desired product as an off-white solid (0.43 g).

WORKUP

后处理

  1. customthe reaction quenched with 5% aqueous sodium metabisulphite (50 ml)
  2. extractionthe product extracted with ethyl acetate (2×100 ml)
  3. dry with materialdried over magnesium sulphate
  4. filtrationfiltered
  5. customthe filtrate evaporated in vacuo
  6. dissolutionThe residue was dissolved in ethyl acetate
  7. customThe solution was evaporated in vacuo