HRID260814

反应详情

EQUATION

反应方程式

HRID 260814 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

HEPAAQ was prepared by a procedure described in Lord, M. W.; Peters, A. T.; J. Chem. Soc., Perkins Trans., 1,(20)2305-8, incorporated herein by reference, with a slight modification. In a 250 mL single-necked round-bottom flask equipped with a reflux condenser was placed 1-chloroanthraquinone (10.5 g), 4-aminophenethyl alcohol (11.2 g), potassium acetate (7.87 g), copper acetate (0.46 g), and nitrobenzene (75 mL). The flask was flushed with nitrogen and then heated to reflux for about 2 hours. The mixture was filtered. The solvent was removed from the filtrate, and the resultant solid was washed with methanol. The product was purified by dissolving the dried filtrate in dichloromethane and chromatographing on a silica column using a 10/90 (v/v) acetone/dichloromethane mixture as the eluent. The solvent was removed from the chromatographed material and dried in vacuo.

WORKUP

后处理

  1. customHEPAAQ was prepared by a procedure
  2. customIn a 250 mL single-necked round-bottom flask equipped with a reflux condenser
  3. customThe flask was flushed with nitrogen
  4. temperatureheated
  5. temperatureto reflux for about 2 hours
  6. filtrationThe mixture was filtered
  7. customThe solvent was removed from the filtrate
  8. washthe resultant solid was washed with methanol
  9. customThe product was purified
  10. dissolutionby dissolving the dried filtrate in dichloromethane
  11. customThe solvent was removed from the chromatographed material
  12. customdried in vacuo