反应 #1463488

反应方程式

nitrobenzene

1-chloroanthraquinone

4-aminophenethyl alcohol

potassium acetate

→

1-[4-[2-hydroxyethyl]phenyl]aminoanthraquinone

反应条件

后处理

1. 1
   其他HEPAAQ was prepared by a procedure
2. 2
   其他In a 250 mL single-necked round-bottom flask equipped with a reflux condenser
3. 3
   其他The flask was flushed with nitrogen
4. 4
   温度heated
5. 5
   温度to reflux for about 2 hours
6. 6
   过滤The resulting mixture was filtered
7. 7
   其他The solvent was removed from the filtrate
8. 8
   洗涤the resultant solid was washed with methanol
9. 9
   其他The product was purified
10. 10
    workup.DISSOLUTIONby dissolving the dried filtrate in dichloromethane
11. 11
    其他The solvent was removed from the chromatographed material
12. 12
    其他dried in vacuo

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 resulting 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.

来源