HRID862615

反应详情

EQUATION

反应方程式

HRID 862615 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of ethyl 2-chloromethyl-6,7-dimethoxy-4-(3,4-dimethoxyphenyl)quinoline-3-carboxylate (3.0 g), m-chloroperbenzoic acid (85%, 2.3 g) and methanol (40 ml) was stirred for 2 hours under reflux. The solvent in the reaction mixture was evaporated under reduced pressure, and the residue was poured into chloroform. The chloroform layer was washed with water and dried over magnesium sulfate. The solvent was evaporated under reduced pressure. The residue was subjected to column chromatography on silica gel. The fractions eluted with chloroform/ethyl acetate (=6/4, v/v) gave ethyl 2-chloromethyl-6,7-dimethoxy-4-(3,4-dimethoxyphenyl)quinoline-3-carboxylate 1-oxide (2.0 g, 65%) which was then recrystallized from acetone-isopropyl ether.

WORKUP

后处理

  1. temperatureunder reflux
  2. customThe solvent in the reaction mixture was evaporated under reduced pressure
  3. additionthe residue was poured into chloroform
  4. washThe chloroform layer was washed with water
  5. dry with materialdried over magnesium sulfate
  6. customThe solvent was evaporated under reduced pressure
  7. washThe fractions eluted with chloroform/ethyl acetate (=6/4, v/v)