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