HRID1087305
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureat reflux for 10 mins
- temperaturethe mixture was heated on a steam bath for a further 10 mins
- customto destroy excess acid chloride
- custom0n evaporation of low-boiling material
- additionthe remaining liquid was diluted with toluene (100ml)
- customseparated by chromatography on a silica gel column
- washNitrobenzene eluted first
- washthe material eluted with a 50:50 mixture of toluene
- customethyl acetate was collected
- customThe solvent was evaporated
- additionethanol was added to the residue, which upon trituration