HRID1087305

反应详情

EQUATION

反应方程式

HRID 1087305 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1-(n-octylsulfonylamino)-8-aminoanthraquinone (0.25g), 1-ethylhexanoyl chloride (0.5g) and nitrobenzene (5ml) were heated at reflux for 10 mins. After addition of methanol (10ml), the mixture was heated on a steam bath for a further 10 mins to destroy excess acid chloride. 0n evaporation of low-boiling material, the remaining liquid was diluted with toluene (100ml) and separated by chromatography on a silica gel column. Nitrobenzene eluted first, and the material eluted with a 50:50 mixture of toluene:ethyl acetate was collected. The solvent was evaporated and ethanol was added to the residue, which upon trituration afforded the product as a yellow solid.

WORKUP

后处理

  1. temperatureat reflux for 10 mins
  2. temperaturethe mixture was heated on a steam bath for a further 10 mins
  3. customto destroy excess acid chloride
  4. custom0n evaporation of low-boiling material
  5. additionthe remaining liquid was diluted with toluene (100ml)
  6. customseparated by chromatography on a silica gel column
  7. washNitrobenzene eluted first
  8. washthe material eluted with a 50:50 mixture of toluene
  9. customethyl acetate was collected
  10. customThe solvent was evaporated
  11. additionethanol was added to the residue, which upon trituration