HRID613566

反应详情

EQUATION

反应方程式

HRID 613566 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 8-(2,6-dichlorobenzoylamino)-4-hydrazinoquinoline (200 mg) in formic acid (4 ml) was added formamide (26 mg), and the mixture was stirred at ambient temperature for 3 hours. The solvent was azeotropically removed with toluene. The residue was diluted with ethyl acetate, washed with water and saturated aqueous sodium bicarbonate solution, dried over magnesium sulfate and concentrated in vacuo. The residual solid was treated with hot ethanol (2 ml), allowed to cool to ambient temperature, filtered and washed with ethanol to give 8-(2,6-dichlorobenzoylamino)-4-(2-formylhydrazino)quinoline (180 mg) as pale yellow crystal.

WORKUP

后处理

  1. customThe solvent was azeotropically removed with toluene
  2. additionThe residue was diluted with ethyl acetate
  3. washwashed with water and saturated aqueous sodium bicarbonate solution
  4. dry with materialdried over magnesium sulfate
  5. concentrationconcentrated in vacuo
  6. additionThe residual solid was treated with hot ethanol (2 ml)
  7. temperatureto cool to ambient temperature
  8. filtrationfiltered
  9. washwashed with ethanol