HRID1684575

反应详情

EQUATION

反应方程式

HRID 1684575 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 2-amino-3',4',4,5-tetramethoxybenzophenone hydrochloride (25.0 g), 2,4-octanedione (10.5 g) and ethanol (500 ml) was stirred under reflux for 2 hours. The solvent was evaporated under reduced pressure. The residue was poured into saturated aqueous sodium bicarbonate solution, and extracted with chloroform. The chloroform layer was washed with water and dried over magnesium sulfate. The chloroform was evaporated, and the residue was subjected to column chromatography on silica gel. The fractions eluted with chloroform-ethanol (20:1, v/v) gave 4-(3,4-dimethoxyphenyl)-6,7-dimethoxy-2-methyl-3-valerylquinoline- This compound was recrystallized from ethanol to give colorless prisms. mp. 119°-120° C.

WORKUP

后处理

  1. temperatureunder reflux for 2 hours
  2. customThe solvent was evaporated under reduced pressure
  3. additionThe residue was poured into saturated aqueous sodium bicarbonate solution
  4. extractionextracted with chloroform
  5. washThe chloroform layer was washed with water
  6. dry with materialdried over magnesium sulfate
  7. customThe chloroform was evaporated
  8. washThe fractions eluted with chloroform-ethanol (20:1