HRID2164708

反应详情

EQUATION

反应方程式

HRID 2164708 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 200 ml of orthodichlorobenzene were added 31.6 g of trans-4-n-butylcyclohexanol, 5.6 g of p-toluenesulfonic acid, and 28 g of 1-amino-4-n-butylanilinoanthraquinone-2-carboxylic acid. The mixture was heated slowly to 110° to 115° C. and maintained at this temperature for 17 hours with stirring. The orthochlorobenzene solution was concentrated to 70 ml under reduced pressure, and 1500 ml of methanol was added. The resulting precipitates was filtered out and then purified by column chromatography wherein silica gel was used as a carrier and chloroform was used as a solvent to obtain 17.3 g of 1-amino-4-n-butylanilinoanthraquinone-2-carboxylic acid-trans-4-n-butylcyclohexyl ester.

WORKUP

后处理

  1. temperatureThe mixture was heated slowly to 110° to 115° C.
  2. temperaturemaintained at this temperature for 17 hours
  3. concentrationThe orthochlorobenzene solution was concentrated to 70 ml under reduced pressure, and 1500 ml of methanol
  4. additionwas added
  5. customThe resulting precipitates
  6. filtrationwas filtered out
  7. custompurified by column chromatography wherein silica gel