HRID1604546

反应详情

EQUATION

反应方程式

HRID 1604546 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

To a solution of ethyl 3,6-dimethylquinoline-2-carboxylate (1.0 g) in tetrachloromethane (10 ml) were added N-bromosuccimide (815 mg) and 2,2'-azobis (2,4-dimethyl-4-methoxyvaleronitrile) at ambient temperature under nitrogen atmosphere, and the mixture was heated at 90° C. for 1 hour. The reaction mixture was poured into 5% sodium thiosulfate solution and extracted with dichloromethane. The organic layer was washed with water, dried over magnesium sulfate, and concentrated in vacuo. The residue was purified by flash chromatography (n-hexane--ethyl acetate) to give ethyl 6-bromomethyl-3-methylquinoline-2-carboxylate (802 mg) as a solid.

WORKUP

后处理

  1. extractionextracted with dichloromethane
  2. washThe organic layer was washed with water
  3. dry with materialdried over magnesium sulfate
  4. concentrationconcentrated in vacuo
  5. customThe residue was purified by flash chromatography (n-hexane--ethyl acetate)